data_complex1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H22 Cd Cl2 N6 O4' _chemical_formula_weight 761.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.9938(19) _cell_length_b 12.6823(16) _cell_length_c 8.2101(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.660(2) _cell_angle_gamma 90.00 _cell_volume 1560.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 0.921 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.818782 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10700 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 28.33 _reflns_number_total 3871 _reflns_number_gt 3025 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELTXL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.2011P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3871 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.0000 0.5000 0.0000 0.03397(9) Uani 1 2 d S . . Cl1 Cl -0.06175(4) 0.57894(5) 0.25966(7) 0.04341(15) Uani 1 1 d . . . N1 N 0.09417(11) 0.65143(14) -0.0340(2) 0.0351(4) Uani 1 1 d . . . N2 N 0.34490(12) 0.52693(15) -0.0686(3) 0.0357(4) Uani 1 1 d . . . N3 N 0.12451(12) 0.41744(15) 0.1523(2) 0.0387(4) Uani 1 1 d . . . O1 O 0.36785(13) 0.78184(16) -0.2217(3) 0.0777(7) Uani 1 1 d . . . O2 O 0.41185(13) 0.28183(15) 0.0936(3) 0.0610(5) Uani 1 1 d . . . C5 C 0.07149(15) 0.74724(18) 0.0165(3) 0.0426(6) Uani 1 1 d . . . H5A H 0.0156 0.7562 0.0608 0.051 Uiso 1 1 calc R . . C4 C 0.12646(17) 0.83377(19) 0.0066(3) 0.0477(6) Uani 1 1 d . . . H4A H 0.1072 0.8998 0.0401 0.057 Uiso 1 1 calc R . . C3 C 0.21020(16) 0.82092(18) -0.0535(3) 0.0435(6) Uani 1 1 d . . . H3A H 0.2486 0.8782 -0.0613 0.052 Uiso 1 1 calc R . . C2 C 0.23697(14) 0.72074(17) -0.1027(3) 0.0346(5) Uani 1 1 d . . . C1 C 0.17549(14) 0.63947(17) -0.0939(3) 0.0347(5) Uani 1 1 d . . . H1A H 0.1916 0.5732 -0.1317 0.042 Uiso 1 1 calc R . . C6 C 0.32720(15) 0.70653(19) -0.1709(3) 0.0449(6) Uani 1 1 d . . . C7 C 0.37045(15) 0.59954(18) -0.1765(3) 0.0390(5) Uani 1 1 d . . . C8 C 0.43832(17) 0.5819(2) -0.2854(3) 0.0503(6) Uani 1 1 d . . . H8A H 0.4542 0.6338 -0.3591 0.060 Uiso 1 1 calc R . . C9 C 0.48145(19) 0.4860(2) -0.2818(4) 0.0549(7) Uani 1 1 d . . . H9A H 0.5266 0.4719 -0.3540 0.066 Uiso 1 1 calc R . . C10 C 0.45686(17) 0.4113(2) -0.1701(3) 0.0490(6) Uani 1 1 d . . . H10A H 0.4857 0.3464 -0.1645 0.059 Uiso 1 1 calc R . . C11 C 0.38846(14) 0.43439(18) -0.0663(3) 0.0371(5) Uani 1 1 d . . . C12 C 0.36309(15) 0.35674(18) 0.0632(3) 0.0408(5) Uani 1 1 d . . . C16 C 0.28027(16) 0.37391(17) 0.1538(3) 0.0394(5) Uani 1 1 d . . . C15 C 0.28015(18) 0.3606(2) 0.3226(3) 0.0502(6) Uani 1 1 d . . . H15A H 0.3319 0.3402 0.3793 0.060 Uiso 1 1 calc R . . C14 C 0.2027(2) 0.3780(2) 0.4037(3) 0.0549(7) Uani 1 1 d . . . H14A H 0.2013 0.3701 0.5162 0.066 Uiso 1 1 calc R . . C13 C 0.12673(17) 0.40752(19) 0.3151(3) 0.0462(6) Uani 1 1 d . . . H13A H 0.0749 0.4211 0.3711 0.055 Uiso 1 1 calc R . . C17 C 0.20008(15) 0.39982(17) 0.0748(3) 0.0374(5) Uani 1 1 d . . . H17B H 0.1990 0.4052 -0.0382 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02557(12) 0.04003(14) 0.03663(14) -0.00159(10) 0.00657(8) -0.00550(9) Cl1 0.0413(3) 0.0535(3) 0.0359(3) -0.0068(3) 0.0080(2) -0.0058(3) N1 0.0278(9) 0.0337(9) 0.0441(11) -0.0002(8) 0.0063(8) -0.0006(7) N2 0.0256(9) 0.0367(9) 0.0449(11) -0.0033(8) 0.0027(8) 0.0005(7) N3 0.0348(10) 0.0390(10) 0.0426(11) 0.0037(9) 0.0050(8) -0.0031(8) O1 0.0453(11) 0.0499(11) 0.139(2) 0.0270(13) 0.0300(12) -0.0084(9) O2 0.0510(11) 0.0526(11) 0.0790(14) 0.0077(10) -0.0055(10) 0.0212(9) C5 0.0346(12) 0.0407(12) 0.0531(15) 0.0014(11) 0.0099(10) 0.0086(10) C4 0.0523(15) 0.0317(12) 0.0595(16) -0.0022(11) 0.0073(12) 0.0062(11) C3 0.0426(13) 0.0301(11) 0.0576(16) 0.0022(11) -0.0012(11) -0.0039(10) C2 0.0290(11) 0.0324(11) 0.0424(12) 0.0035(9) 0.0009(9) -0.0015(8) C1 0.0297(11) 0.0291(10) 0.0453(13) -0.0012(9) 0.0034(9) -0.0012(8) C6 0.0303(12) 0.0426(13) 0.0620(16) 0.0076(12) 0.0054(11) -0.0053(10) C7 0.0281(11) 0.0428(12) 0.0462(13) -0.0021(10) 0.0044(9) -0.0036(9) C8 0.0413(14) 0.0638(17) 0.0463(15) 0.0008(13) 0.0107(11) -0.0040(13) C9 0.0400(14) 0.073(2) 0.0529(17) -0.0158(14) 0.0166(12) 0.0054(12) C10 0.0381(13) 0.0542(15) 0.0547(16) -0.0171(13) 0.0018(11) 0.0112(11) C11 0.0268(11) 0.0416(12) 0.0426(13) -0.0096(10) -0.0037(9) 0.0027(9) C12 0.0360(12) 0.0383(12) 0.0477(14) -0.0045(10) -0.0074(10) 0.0047(10) C16 0.0416(13) 0.0315(11) 0.0449(14) 0.0025(10) -0.0018(10) 0.0016(10) C15 0.0536(16) 0.0466(14) 0.0501(15) 0.0109(12) -0.0057(12) 0.0077(12) C14 0.0665(18) 0.0577(16) 0.0405(14) 0.0120(12) 0.0019(13) 0.0050(14) C13 0.0490(14) 0.0425(13) 0.0478(14) 0.0069(11) 0.0141(11) -0.0022(11) C17 0.0359(12) 0.0370(11) 0.0394(12) 0.0013(10) 0.0010(9) -0.0010(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.4047(17) 3_565 ? Cd1 N1 2.4047(17) . ? Cd1 N3 2.4515(19) 3_565 ? Cd1 N3 2.4515(19) . ? Cd1 Cl1 2.5531(6) 3_565 ? Cd1 Cl1 2.5531(6) . ? N1 C5 1.331(3) . ? N1 C1 1.337(3) . ? N2 C7 1.341(3) . ? N2 C11 1.343(3) . ? N3 C17 1.334(3) . ? N3 C13 1.342(3) . ? O1 C6 1.213(3) . ? O2 C12 1.220(3) . ? C5 C4 1.376(3) . ? C5 H5A 0.9300 . ? C4 C3 1.372(4) . ? C4 H4A 0.9300 . ? C3 C2 1.396(3) . ? C3 H3A 0.9300 . ? C2 C1 1.386(3) . ? C2 C6 1.490(3) . ? C1 H1A 0.9300 . ? C6 C7 1.505(3) . ? C7 C8 1.392(3) . ? C8 C9 1.377(4) . ? C8 H8A 0.9300 . ? C9 C10 1.376(4) . ? C9 H9A 0.9300 . ? C10 C11 1.384(3) . ? C10 H10A 0.9300 . ? C11 C12 1.506(3) . ? C12 C16 1.482(3) . ? C16 C17 1.389(3) . ? C16 C15 1.396(3) . ? C15 C14 1.372(4) . ? C15 H15A 0.9300 . ? C14 C13 1.385(4) . ? C14 H14A 0.9300 . ? C13 H13A 0.9300 . ? C17 H17B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 180.00(9) 3_565 . ? N1 Cd1 N3 87.66(6) 3_565 3_565 ? N1 Cd1 N3 92.34(6) . 3_565 ? N1 Cd1 N3 92.34(6) 3_565 . ? N1 Cd1 N3 87.66(6) . . ? N3 Cd1 N3 180.00(8) 3_565 . ? N1 Cd1 Cl1 90.69(5) 3_565 3_565 ? N1 Cd1 Cl1 89.31(5) . 3_565 ? N3 Cd1 Cl1 91.76(5) 3_565 3_565 ? N3 Cd1 Cl1 88.24(5) . 3_565 ? N1 Cd1 Cl1 89.31(5) 3_565 . ? N1 Cd1 Cl1 90.69(5) . . ? N3 Cd1 Cl1 88.24(5) 3_565 . ? N3 Cd1 Cl1 91.76(5) . . ? Cl1 Cd1 Cl1 180.0 3_565 . ? C5 N1 C1 117.53(19) . . ? C5 N1 Cd1 122.46(15) . . ? C1 N1 Cd1 119.80(14) . . ? C7 N2 C11 117.5(2) . . ? C17 N3 C13 117.5(2) . . ? C17 N3 Cd1 118.22(15) . . ? C13 N3 Cd1 123.00(16) . . ? N1 C5 C4 123.4(2) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? C3 C4 C5 118.8(2) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? C4 C3 C2 119.1(2) . . ? C4 C3 H3A 120.5 . . ? C2 C3 H3A 120.5 . . ? C1 C2 C3 117.7(2) . . ? C1 C2 C6 122.8(2) . . ? C3 C2 C6 119.4(2) . . ? N1 C1 C2 123.4(2) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? O1 C6 C2 120.3(2) . . ? O1 C6 C7 118.6(2) . . ? C2 C6 C7 121.1(2) . . ? N2 C7 C8 122.8(2) . . ? N2 C7 C6 117.9(2) . . ? C8 C7 C6 119.2(2) . . ? C9 C8 C7 118.7(3) . . ? C9 C8 H8A 120.7 . . ? C7 C8 H8A 120.7 . . ? C10 C9 C8 119.2(3) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? C9 C10 C11 118.9(2) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? N2 C11 C10 123.0(2) . . ? N2 C11 C12 116.7(2) . . ? C10 C11 C12 120.2(2) . . ? O2 C12 C16 121.2(2) . . ? O2 C12 C11 119.4(2) . . ? C16 C12 C11 119.39(19) . . ? C17 C16 C15 117.8(2) . . ? C17 C16 C12 121.8(2) . . ? C15 C16 C12 120.4(2) . . ? C14 C15 C16 119.2(2) . . ? C14 C15 H15A 120.4 . . ? C16 C15 H15A 120.4 . . ? C15 C14 C13 118.9(3) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? N3 C13 C14 123.0(2) . . ? N3 C13 H13A 118.5 . . ? C14 C13 H13A 118.5 . . ? N3 C17 C16 123.5(2) . . ? N3 C17 H17B 118.2 . . ? C16 C17 H17B 118.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cd1 N1 C5 170(100) 3_565 . . . ? N3 Cd1 N1 C5 57.71(18) 3_565 . . . ? N3 Cd1 N1 C5 -122.29(18) . . . . ? Cl1 Cd1 N1 C5 149.45(18) 3_565 . . . ? Cl1 Cd1 N1 C5 -30.55(18) . . . . ? N1 Cd1 N1 C1 -15(100) 3_565 . . . ? N3 Cd1 N1 C1 -127.66(17) 3_565 . . . ? N3 Cd1 N1 C1 52.34(17) . . . . ? Cl1 Cd1 N1 C1 -35.92(16) 3_565 . . . ? Cl1 Cd1 N1 C1 144.08(16) . . . . ? N1 Cd1 N3 C17 117.89(16) 3_565 . . . ? N1 Cd1 N3 C17 -62.11(16) . . . . ? N3 Cd1 N3 C17 51(100) 3_565 . . . ? Cl1 Cd1 N3 C17 27.27(16) 3_565 . . . ? Cl1 Cd1 N3 C17 -152.73(16) . . . . ? N1 Cd1 N3 C13 -75.14(18) 3_565 . . . ? N1 Cd1 N3 C13 104.86(18) . . . . ? N3 Cd1 N3 C13 -142(100) 3_565 . . . ? Cl1 Cd1 N3 C13 -165.76(18) 3_565 . . . ? Cl1 Cd1 N3 C13 14.24(18) . . . . ? C1 N1 C5 C4 1.5(4) . . . . ? Cd1 N1 C5 C4 176.22(19) . . . . ? N1 C5 C4 C3 -2.1(4) . . . . ? C5 C4 C3 C2 0.0(4) . . . . ? C4 C3 C2 C1 2.5(4) . . . . ? C4 C3 C2 C6 178.9(2) . . . . ? C5 N1 C1 C2 1.3(3) . . . . ? Cd1 N1 C1 C2 -173.59(16) . . . . ? C3 C2 C1 N1 -3.3(3) . . . . ? C6 C2 C1 N1 -179.5(2) . . . . ? C1 C2 C6 O1 157.7(3) . . . . ? C3 C2 C6 O1 -18.6(4) . . . . ? C1 C2 C6 C7 -23.2(4) . . . . ? C3 C2 C6 C7 160.6(2) . . . . ? C11 N2 C7 C8 1.0(3) . . . . ? C11 N2 C7 C6 -175.1(2) . . . . ? O1 C6 C7 N2 154.3(3) . . . . ? C2 C6 C7 N2 -24.8(3) . . . . ? O1 C6 C7 C8 -21.9(4) . . . . ? C2 C6 C7 C8 158.9(2) . . . . ? N2 C7 C8 C9 -0.4(4) . . . . ? C6 C7 C8 C9 175.7(2) . . . . ? C7 C8 C9 C10 -0.6(4) . . . . ? C8 C9 C10 C11 1.0(4) . . . . ? C7 N2 C11 C10 -0.6(3) . . . . ? C7 N2 C11 C12 175.9(2) . . . . ? C9 C10 C11 N2 -0.4(4) . . . . ? C9 C10 C11 C12 -176.8(2) . . . . ? N2 C11 C12 O2 -164.8(2) . . . . ? C10 C11 C12 O2 11.8(3) . . . . ? N2 C11 C12 C16 14.0(3) . . . . ? C10 C11 C12 C16 -169.4(2) . . . . ? O2 C12 C16 C17 -134.8(2) . . . . ? C11 C12 C16 C17 46.5(3) . . . . ? O2 C12 C16 C15 42.9(3) . . . . ? C11 C12 C16 C15 -135.8(2) . . . . ? C17 C16 C15 C14 -2.8(4) . . . . ? C12 C16 C15 C14 179.4(2) . . . . ? C16 C15 C14 C13 0.5(4) . . . . ? C17 N3 C13 C14 -1.4(4) . . . . ? Cd1 N3 C13 C14 -168.45(19) . . . . ? C15 C14 C13 N3 1.7(4) . . . . ? C13 N3 C17 C16 -1.2(3) . . . . ? Cd1 N3 C17 C16 166.49(17) . . . . ? C15 C16 C17 N3 3.3(3) . . . . ? C12 C16 C17 N3 -178.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.652 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.070 ########################end############################ data_complex2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H29 Cd N8 O13.50' _chemical_formula_weight 878.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.741(3) _cell_length_b 15.1729(16) _cell_length_c 20.697(2) _cell_angle_alpha 90.00 _cell_angle_beta 125.529(2) _cell_angle_gamma 90.00 _cell_volume 7856.5(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 0.629 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.738062 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21026 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6889 _reflns_number_gt 4676 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker 2007)' _computing_cell_refinement 'APEX2 and SAINT (Bruker 2007)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1214P)^2^+23.4343P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6889 _refine_ls_number_parameters 540 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1006 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.2285 _refine_ls_wR_factor_gt 0.1929 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.7500 0.7500 0.5000 0.0653(3) Uani 1 2 d S . . Cd2 Cd 0.5000 0.5000 0.5000 0.1005(4) Uani 1 2 d S . . N1 N 0.8063(2) 0.6582(3) 0.4873(3) 0.0678(14) Uani 1 1 d . . . C1 C 0.8141(3) 0.5764(5) 0.5133(5) 0.084(2) Uani 1 1 d . . . H1A H 0.8027 0.5610 0.5448 0.101 Uiso 1 1 calc R . . C2 C 0.8379(4) 0.5128(5) 0.4970(5) 0.088(2) Uani 1 1 d . . . H2A H 0.8432 0.4563 0.5179 0.105 Uiso 1 1 calc R . . C3 C 0.8538(3) 0.5339(4) 0.4491(4) 0.0712(17) Uani 1 1 d . . . H3A H 0.8700 0.4923 0.4366 0.085 Uiso 1 1 calc R . . C4 C 0.8450(2) 0.6187(4) 0.4202(3) 0.0579(14) Uani 1 1 d . . . C5 C 0.8229(2) 0.6793(4) 0.4425(4) 0.0591(14) Uani 1 1 d . . . H5A H 0.8194 0.7373 0.4256 0.071 Uiso 1 1 calc R . . C6 C 0.8617(3) 0.6432(4) 0.3670(4) 0.0656(16) Uani 1 1 d . . . O1 O 0.8999(2) 0.6058(4) 0.3751(4) 0.0962(17) Uani 1 1 d . . . N2 N 0.7820(2) 0.7298(3) 0.2781(3) 0.0557(12) Uani 1 1 d . . . C7 C 0.8317(3) 0.7111(4) 0.3036(4) 0.0580(14) Uani 1 1 d . . . C8 C 0.8565(3) 0.7468(5) 0.2706(5) 0.0753(19) Uani 1 1 d . . . H8A H 0.8912 0.7315 0.2895 0.090 Uiso 1 1 calc R . . C9 C 0.8270(4) 0.8068(5) 0.2080(5) 0.082(2) Uani 1 1 d . . . H9A H 0.8422 0.8335 0.1850 0.098 Uiso 1 1 calc R . . C10 C 0.7762(3) 0.8250(4) 0.1817(4) 0.0740(19) Uani 1 1 d . . . H10A H 0.7557 0.8635 0.1394 0.089 Uiso 1 1 calc R . . C11 C 0.7547(3) 0.7860(4) 0.2180(3) 0.0562(14) Uani 1 1 d . . . C12 C 0.6968(3) 0.8036(4) 0.1848(3) 0.0612(15) Uani 1 1 d . . . O2 O 0.66706(19) 0.8297(3) 0.1166(2) 0.0759(13) Uani 1 1 d . . . N3 N 0.6904(2) 0.7777(4) 0.3599(4) 0.0713(14) Uani 1 1 d . . . C13 C 0.7080(3) 0.7928(4) 0.3156(4) 0.0612(15) Uani 1 1 d . . . H13A H 0.7439 0.8068 0.3415 0.073 Uiso 1 1 calc R . . C14 C 0.6765(3) 0.7890(4) 0.2331(4) 0.0645(16) Uani 1 1 d . . . C15 C 0.6221(3) 0.7708(6) 0.1956(5) 0.094(2) Uani 1 1 d . . . H15A H 0.5988 0.7691 0.1405 0.112 Uiso 1 1 calc R . . C16 C 0.6038(4) 0.7558(7) 0.2407(6) 0.106(3) Uani 1 1 d . . . H16A H 0.5679 0.7433 0.2169 0.127 Uiso 1 1 calc R . . C17 C 0.6392(3) 0.7592(6) 0.3219(6) 0.092(2) Uani 1 1 d . . . H17A H 0.6262 0.7477 0.3520 0.110 Uiso 1 1 calc R . . N4 N 0.4747(2) 0.6264(6) 0.5368(4) 0.090(2) Uani 1 1 d . . . C18 C 0.4275(3) 0.6313(6) 0.5269(4) 0.0752(19) Uani 1 1 d . . . H18A H 0.4076 0.5801 0.5154 0.090 Uiso 1 1 calc R . . C19 C 0.4075(3) 0.7107(5) 0.5331(4) 0.0703(18) Uani 1 1 d . . . C20 C 0.4385(3) 0.7852(7) 0.5524(5) 0.092(2) Uani 1 1 d . . . H20A H 0.4266 0.8394 0.5574 0.110 Uiso 1 1 calc R . . C21 C 0.4857(4) 0.7783(8) 0.5636(6) 0.108(3) Uani 1 1 d . . . H21A H 0.5072 0.8277 0.5767 0.130 Uiso 1 1 calc R . . C22 C 0.5023(3) 0.6970(10) 0.5555(5) 0.112(4) Uani 1 1 d . . . H22A H 0.5355 0.6934 0.5643 0.135 Uiso 1 1 calc R . . C23 C 0.3554(3) 0.7175(5) 0.5208(4) 0.0759(19) Uani 1 1 d . . . O3 O 0.3478(3) 0.7746(5) 0.5550(4) 0.110(2) Uani 1 1 d . . . N5 N 0.31223(19) 0.6177(3) 0.4081(3) 0.0587(12) Uani 1 1 d . . . C24 C 0.3101(3) 0.6571(4) 0.4630(4) 0.0660(17) Uani 1 1 d . . . C25 C 0.2662(4) 0.6491(5) 0.4662(6) 0.086(2) Uani 1 1 d . . . H25A H 0.2661 0.6762 0.5065 0.104 Uiso 1 1 calc R . . C26 C 0.2229(4) 0.6001(5) 0.4086(7) 0.097(3) Uani 1 1 d . . . H26A H 0.1926 0.5961 0.4084 0.116 Uiso 1 1 calc R . . C28 C 0.2707(3) 0.5681(4) 0.3545(4) 0.0661(17) Uani 1 1 d . . . O4 O 0.2310(2) 0.4966(3) 0.2313(4) 0.0971(18) Uani 1 1 d . . . N6 N 0.4170(2) 0.5006(4) 0.3741(3) 0.0768(16) Uani 1 1 d . . . C29 C 0.2717(3) 0.5264(4) 0.2894(5) 0.0716(18) Uani 1 1 d . . . C30 C 0.3706(3) 0.5047(4) 0.3660(4) 0.0676(17) Uani 1 1 d . . . H30A H 0.3709 0.4928 0.4103 0.081 Uiso 1 1 calc R . . C31 C 0.3235(3) 0.5251(4) 0.2975(4) 0.0661(16) Uani 1 1 d . . . C32 C 0.3224(3) 0.5383(5) 0.2302(4) 0.080(2) Uani 1 1 d . . . H32A H 0.2904 0.5511 0.1818 0.096 Uiso 1 1 calc R . . C33 C 0.3692(4) 0.5321(6) 0.2360(5) 0.091(2) Uani 1 1 d . . . H33A H 0.3692 0.5392 0.1914 0.109 Uiso 1 1 calc R . . C34 C 0.4151(4) 0.5156(6) 0.3076(5) 0.089(2) Uani 1 1 d . . . H34A H 0.4469 0.5144 0.3118 0.107 Uiso 1 1 calc R . . C27 C 0.2244(3) 0.5583(5) 0.3531(6) 0.088(2) Uani 1 1 d . . . H27A H 0.1958 0.5238 0.3147 0.105 Uiso 1 1 calc R . . N7 N 0.6752(3) 0.5844(4) 0.4834(4) 0.0872(18) Uani 1 1 d U . . O5 O 0.6950(3) 0.6190(5) 0.4547(5) 0.140(3) Uani 1 1 d U . . O6 O 0.6858(4) 0.6112(5) 0.5459(5) 0.152(3) Uani 1 1 d U . . O7 O 0.6441(3) 0.5279(5) 0.4508(4) 0.118(2) Uani 1 1 d U . . N8 N 0.5580(6) 0.6508(9) 0.4522(8) 0.190(4) Uani 1 1 d DU . . O9 O 0.5613(6) 0.6873(11) 0.4009(8) 0.251(6) Uani 1 1 d DU . . O8 O 0.5361(3) 0.5793(6) 0.4448(5) 0.145(3) Uani 1 1 d DU . . O10 O 0.5876(5) 0.6818(10) 0.5206(8) 0.239(6) Uani 1 1 d DU . . O1W O 0.4628(10) 0.306(3) 0.2359(9) 0.30(2) Uani 0.50 1 d P . . O1W' O 0.4608(17) 0.167(3) 0.2316(14) 0.47(4) Uani 0.50 1 d P . . O3W O 0.5053(12) 1.034(3) 0.5482(17) 0.202(13) Uani 0.50 1 d P . . O3W' O 0.5262(7) 1.0562(15) 0.522(3) 0.212(14) Uani 0.50 1 d P . . O2W O 0.5438(9) 0.836(4) 0.368(3) 0.67(7) Uani 0.60 1 d P . . O2W' O 0.5000 0.575(3) 0.2500 0.319(17) Uani 0.80 2 d SP . . O4W O 0.4815(14) 0.987(3) 0.635(3) 0.49(5) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0775(5) 0.0657(4) 0.0668(4) 0.0076(3) 0.0500(4) 0.0148(3) Cd2 0.0567(5) 0.1770(10) 0.0735(5) 0.0096(5) 0.0411(4) 0.0430(5) N1 0.089(4) 0.055(3) 0.073(3) 0.014(3) 0.055(3) 0.015(3) C1 0.118(6) 0.064(4) 0.109(6) 0.035(4) 0.088(5) 0.033(4) C2 0.118(7) 0.066(4) 0.107(6) 0.028(4) 0.081(6) 0.025(4) C3 0.074(4) 0.059(4) 0.084(5) 0.007(3) 0.048(4) 0.014(3) C4 0.051(3) 0.063(4) 0.059(3) 0.006(3) 0.031(3) 0.007(3) C5 0.063(4) 0.049(3) 0.064(3) 0.006(3) 0.036(3) 0.007(3) C6 0.058(4) 0.068(4) 0.071(4) -0.003(3) 0.037(3) 0.004(3) O1 0.080(3) 0.115(4) 0.121(4) 0.028(3) 0.074(3) 0.033(3) N2 0.063(3) 0.052(3) 0.053(3) -0.004(2) 0.034(3) -0.004(2) C7 0.063(4) 0.056(3) 0.062(3) -0.005(3) 0.041(3) -0.007(3) C8 0.079(5) 0.077(4) 0.081(5) -0.013(4) 0.053(4) -0.011(4) C9 0.099(6) 0.086(5) 0.077(5) -0.002(4) 0.060(5) -0.011(4) C10 0.100(6) 0.058(4) 0.063(4) -0.001(3) 0.046(4) -0.006(4) C11 0.072(4) 0.047(3) 0.051(3) -0.010(3) 0.036(3) -0.010(3) C12 0.071(4) 0.046(3) 0.047(3) -0.003(2) 0.023(3) 0.000(3) O2 0.083(3) 0.067(3) 0.050(2) 0.003(2) 0.023(2) 0.002(2) N3 0.064(4) 0.082(4) 0.076(4) 0.011(3) 0.045(3) 0.015(3) C13 0.056(3) 0.060(4) 0.058(3) 0.002(3) 0.028(3) 0.006(3) C14 0.062(4) 0.053(3) 0.059(4) 0.002(3) 0.025(3) 0.003(3) C15 0.056(4) 0.119(7) 0.079(5) 0.011(4) 0.024(4) 0.011(4) C16 0.061(5) 0.138(8) 0.106(7) 0.014(6) 0.042(5) 0.003(5) C17 0.070(5) 0.113(6) 0.103(6) 0.018(5) 0.056(5) 0.021(4) N4 0.045(3) 0.145(6) 0.073(4) -0.005(4) 0.030(3) 0.011(4) C18 0.062(4) 0.108(6) 0.060(4) 0.010(4) 0.039(3) 0.027(4) C19 0.059(4) 0.098(5) 0.049(3) 0.013(3) 0.029(3) 0.022(4) C20 0.071(5) 0.105(6) 0.070(5) 0.013(4) 0.025(4) 0.004(5) C21 0.072(6) 0.139(9) 0.095(6) 0.015(6) 0.039(5) -0.009(6) C22 0.052(5) 0.206(13) 0.077(5) 0.010(7) 0.036(4) 0.010(7) C23 0.076(5) 0.093(5) 0.070(4) 0.012(4) 0.049(4) 0.027(4) O3 0.112(5) 0.133(5) 0.106(4) -0.018(4) 0.075(4) 0.025(4) N5 0.049(3) 0.057(3) 0.071(3) 0.019(2) 0.036(3) 0.017(2) C24 0.073(4) 0.072(4) 0.079(4) 0.028(3) 0.059(4) 0.033(3) C25 0.091(6) 0.082(5) 0.122(6) 0.040(5) 0.082(6) 0.036(5) C26 0.099(6) 0.071(5) 0.173(9) 0.037(6) 0.109(7) 0.025(5) C28 0.056(4) 0.050(3) 0.094(5) 0.019(3) 0.045(4) 0.014(3) O4 0.058(3) 0.081(3) 0.116(4) -0.019(3) 0.031(3) -0.004(2) N6 0.058(3) 0.111(5) 0.066(3) 0.003(3) 0.038(3) 0.019(3) C29 0.055(4) 0.055(4) 0.088(5) 0.014(3) 0.032(4) 0.011(3) C30 0.058(4) 0.082(4) 0.068(4) 0.005(3) 0.040(3) 0.017(3) C31 0.063(4) 0.059(4) 0.067(4) 0.000(3) 0.033(3) 0.003(3) C32 0.080(5) 0.069(4) 0.063(4) 0.001(3) 0.026(4) -0.003(4) C33 0.097(6) 0.111(6) 0.070(5) -0.005(4) 0.052(5) -0.010(5) C34 0.085(6) 0.114(6) 0.089(6) 0.002(5) 0.062(5) 0.011(4) C27 0.066(4) 0.061(4) 0.141(7) 0.026(4) 0.063(5) 0.009(3) N7 0.098(4) 0.054(3) 0.085(4) 0.010(3) 0.039(4) -0.010(3) O5 0.116(5) 0.120(5) 0.151(6) 0.022(4) 0.059(4) -0.028(4) O6 0.190(8) 0.105(5) 0.097(5) -0.016(4) 0.047(5) 0.008(5) O7 0.131(6) 0.098(4) 0.122(5) -0.003(4) 0.071(4) -0.032(4) N8 0.181(8) 0.241(10) 0.199(8) -0.005(8) 0.139(7) -0.020(7) O9 0.240(11) 0.308(15) 0.269(13) 0.011(12) 0.184(10) -0.019(11) O8 0.137(6) 0.177(8) 0.176(6) -0.011(6) 0.121(5) -0.026(5) O10 0.182(11) 0.289(13) 0.227(12) -0.061(11) 0.108(10) -0.022(10) O1W 0.28(3) 0.57(5) 0.065(9) 0.097(18) 0.104(15) 0.27(3) O1W' 0.64(8) 0.63(7) 0.111(19) 0.19(3) 0.20(4) 0.48(7) O3W 0.119(17) 0.30(4) 0.178(19) 0.10(2) 0.083(16) 0.08(2) O3W' 0.081(12) 0.144(15) 0.36(4) 0.10(2) 0.102(19) 0.014(11) O2W 0.094(14) 0.86(10) 0.65(8) -0.60(8) -0.01(3) 0.06(3) O2W' 0.30(3) 0.44(5) 0.39(4) 0.000 0.30(4) 0.000 O4W 0.21(3) 0.43(6) 0.33(5) -0.25(5) -0.13(3) 0.17(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.354(5) . ? Cd1 N1 2.354(5) 7_666 ? Cd1 N3 2.402(6) . ? Cd1 N3 2.402(6) 7_666 ? Cd1 O5 2.418(7) . ? Cd1 O5 2.418(7) 7_666 ? Cd2 O8 2.335(7) 5_666 ? Cd2 O8 2.335(7) . ? Cd2 N4 2.357(7) 5_666 ? Cd2 N4 2.357(7) . ? Cd2 N6 2.361(6) . ? Cd2 N6 2.361(6) 5_666 ? N1 C1 1.320(8) . ? N1 C5 1.330(8) . ? C1 C2 1.366(10) . ? C1 H1A 0.9300 . ? C2 C3 1.375(10) . ? C2 H2A 0.9300 . ? C3 C4 1.377(9) . ? C3 H3A 0.9300 . ? C4 C5 1.373(8) . ? C4 C6 1.507(9) . ? C5 H5A 0.9300 . ? C6 O1 1.223(7) . ? C6 C7 1.492(9) . ? N2 C7 1.326(8) . ? N2 C11 1.329(8) . ? C7 C8 1.393(9) . ? C8 C9 1.401(11) . ? C8 H8A 0.9300 . ? C9 C10 1.351(11) . ? C9 H9A 0.9300 . ? C10 C11 1.387(9) . ? C10 H10A 0.9300 . ? C11 C12 1.514(9) . ? C12 O2 1.219(7) . ? C12 C14 1.469(9) . ? N3 C17 1.318(10) . ? N3 C13 1.328(8) . ? C13 C14 1.391(9) . ? C13 H13A 0.9300 . ? C14 C15 1.402(10) . ? C15 C16 1.361(13) . ? C15 H15A 0.9300 . ? C16 C17 1.373(14) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? N4 C22 1.279(14) . ? N4 C18 1.344(9) . ? C18 C19 1.391(10) . ? C18 H18A 0.9300 . ? C19 C20 1.379(12) . ? C19 C23 1.474(10) . ? C20 C21 1.334(13) . ? C20 H20A 0.9300 . ? C21 C22 1.381(16) . ? C21 H21A 0.9300 . ? C22 H22A 0.9300 . ? C23 O3 1.224(9) . ? C23 C24 1.508(11) . ? N5 C24 1.319(8) . ? N5 C28 1.335(8) . ? C24 C25 1.393(10) . ? C25 C26 1.379(13) . ? C25 H25A 0.9300 . ? C26 C27 1.335(12) . ? C26 H26A 0.9300 . ? C28 C27 1.415(9) . ? C28 C29 1.507(10) . ? O4 C29 1.212(9) . ? N6 C30 1.336(8) . ? N6 C34 1.362(10) . ? C29 C31 1.500(10) . ? C30 C31 1.348(9) . ? C30 H30A 0.9300 . ? C31 C32 1.387(10) . ? C32 C33 1.375(12) . ? C32 H32A 0.9300 . ? C33 C34 1.350(12) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C27 H27A 0.9300 . ? N7 O7 1.165(9) . ? N7 O5 1.191(9) . ? N7 O6 1.206(10) . ? N8 O8 1.238(9) . ? N8 O10 1.247(9) . ? N8 O9 1.253(9) . ? O3W O3W' 1.10(3) . ? O3W O3W' 1.81(4) 5_676 ? O3W' O3W 1.81(4) 5_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 N1 180.0(3) . 7_666 ? N1 Cd1 N3 93.63(19) . . ? N1 Cd1 N3 86.37(19) 7_666 . ? N1 Cd1 N3 86.37(19) . 7_666 ? N1 Cd1 N3 93.63(19) 7_666 7_666 ? N3 Cd1 N3 180.000(1) . 7_666 ? N1 Cd1 O5 82.2(3) . . ? N1 Cd1 O5 97.8(3) 7_666 . ? N3 Cd1 O5 78.7(2) . . ? N3 Cd1 O5 101.3(2) 7_666 . ? N1 Cd1 O5 97.8(3) . 7_666 ? N1 Cd1 O5 82.2(3) 7_666 7_666 ? N3 Cd1 O5 101.3(2) . 7_666 ? N3 Cd1 O5 78.7(2) 7_666 7_666 ? O5 Cd1 O5 180.000(1) . 7_666 ? O8 Cd2 O8 180.0(3) 5_666 . ? O8 Cd2 N4 94.5(3) 5_666 5_666 ? O8 Cd2 N4 85.5(3) . 5_666 ? O8 Cd2 N4 85.5(3) 5_666 . ? O8 Cd2 N4 94.5(3) . . ? N4 Cd2 N4 180.000(2) 5_666 . ? O8 Cd2 N6 91.5(3) 5_666 . ? O8 Cd2 N6 88.5(3) . . ? N4 Cd2 N6 89.7(2) 5_666 . ? N4 Cd2 N6 90.3(2) . . ? O8 Cd2 N6 88.5(3) 5_666 5_666 ? O8 Cd2 N6 91.5(3) . 5_666 ? N4 Cd2 N6 90.3(2) 5_666 5_666 ? N4 Cd2 N6 89.7(2) . 5_666 ? N6 Cd2 N6 180.000(1) . 5_666 ? C1 N1 C5 117.3(6) . . ? C1 N1 Cd1 118.8(4) . . ? C5 N1 Cd1 122.8(4) . . ? N1 C1 C2 124.0(7) . . ? N1 C1 H1A 118.0 . . ? C2 C1 H1A 118.0 . . ? C1 C2 C3 118.7(6) . . ? C1 C2 H2A 120.7 . . ? C3 C2 H2A 120.7 . . ? C2 C3 C4 118.0(6) . . ? C2 C3 H3A 121.0 . . ? C4 C3 H3A 121.0 . . ? C5 C4 C3 119.3(6) . . ? C5 C4 C6 121.7(5) . . ? C3 C4 C6 118.9(6) . . ? N1 C5 C4 122.6(6) . . ? N1 C5 H5A 118.7 . . ? C4 C5 H5A 118.7 . . ? O1 C6 C7 119.7(6) . . ? O1 C6 C4 119.4(6) . . ? C7 C6 C4 120.9(5) . . ? C7 N2 C11 117.7(5) . . ? N2 C7 C8 123.5(6) . . ? N2 C7 C6 118.6(5) . . ? C8 C7 C6 117.7(6) . . ? C7 C8 C9 117.6(7) . . ? C7 C8 H8A 121.2 . . ? C9 C8 H8A 121.2 . . ? C10 C9 C8 118.6(7) . . ? C10 C9 H9A 120.7 . . ? C8 C9 H9A 120.7 . . ? C9 C10 C11 119.9(7) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? N2 C11 C10 122.7(6) . . ? N2 C11 C12 118.3(5) . . ? C10 C11 C12 118.9(6) . . ? O2 C12 C14 120.4(6) . . ? O2 C12 C11 118.4(6) . . ? C14 C12 C11 121.1(5) . . ? C17 N3 C13 116.7(7) . . ? C17 N3 Cd1 119.4(5) . . ? C13 N3 Cd1 122.2(4) . . ? N3 C13 C14 124.7(6) . . ? N3 C13 H13A 117.6 . . ? C14 C13 H13A 117.6 . . ? C13 C14 C15 116.2(7) . . ? C13 C14 C12 124.2(6) . . ? C15 C14 C12 119.7(6) . . ? C16 C15 C14 119.3(8) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C15 C16 C17 119.0(8) . . ? C15 C16 H16A 120.5 . . ? C17 C16 H16A 120.5 . . ? N3 C17 C16 124.0(8) . . ? N3 C17 H17A 118.0 . . ? C16 C17 H17A 118.0 . . ? C22 N4 C18 117.9(8) . . ? C22 N4 Cd2 119.6(6) . . ? C18 N4 Cd2 121.7(6) . . ? N4 C18 C19 121.9(8) . . ? N4 C18 H18A 119.1 . . ? C19 C18 H18A 119.1 . . ? C20 C19 C18 118.0(7) . . ? C20 C19 C23 119.4(7) . . ? C18 C19 C23 122.6(8) . . ? C21 C20 C19 119.0(10) . . ? C21 C20 H20A 120.5 . . ? C19 C20 H20A 120.5 . . ? C20 C21 C22 119.3(10) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? N4 C22 C21 123.9(8) . . ? N4 C22 H22A 118.0 . . ? C21 C22 H22A 118.0 . . ? O3 C23 C19 120.2(8) . . ? O3 C23 C24 119.4(7) . . ? C19 C23 C24 120.4(6) . . ? C24 N5 C28 117.9(6) . . ? N5 C24 C25 122.4(8) . . ? N5 C24 C23 118.2(6) . . ? C25 C24 C23 119.3(7) . . ? C26 C25 C24 118.7(8) . . ? C26 C25 H25A 120.6 . . ? C24 C25 H25A 120.6 . . ? C27 C26 C25 120.1(7) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? N5 C28 C27 122.8(7) . . ? N5 C28 C29 118.2(6) . . ? C27 C28 C29 118.8(7) . . ? C30 N6 C34 116.7(6) . . ? C30 N6 Cd2 121.9(5) . . ? C34 N6 Cd2 119.9(5) . . ? O4 C29 C31 121.6(7) . . ? O4 C29 C28 119.8(7) . . ? C31 C29 C28 118.6(6) . . ? N6 C30 C31 124.0(7) . . ? N6 C30 H30A 118.0 . . ? C31 C30 H30A 118.0 . . ? C30 C31 C32 118.3(7) . . ? C30 C31 C29 122.8(6) . . ? C32 C31 C29 118.7(6) . . ? C33 C32 C31 119.2(7) . . ? C33 C32 H32A 120.4 . . ? C31 C32 H32A 120.4 . . ? C34 C33 C32 118.8(8) . . ? C34 C33 H33A 120.6 . . ? C32 C33 H33A 120.6 . . ? C33 C34 N6 122.9(8) . . ? C33 C34 H34A 118.5 . . ? N6 C34 H34A 118.5 . . ? C26 C27 C28 118.0(8) . . ? C26 C27 H27A 121.0 . . ? C28 C27 H27A 121.0 . . ? O7 N7 O5 121.5(9) . . ? O7 N7 O6 119.2(9) . . ? O5 N7 O6 119.2(9) . . ? N7 O5 Cd1 127.8(7) . . ? O8 N8 O10 117.3(11) . . ? O8 N8 O9 126.0(11) . . ? O10 N8 O9 115.4(11) . . ? N8 O8 Cd2 140.3(8) . . ? O3W' O3W O3W' 92(3) . 5_676 ? O3W O3W' O3W 88(3) . 5_676 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cd1 N1 C1 147(100) 7_666 . . . ? N3 Cd1 N1 C1 -121.6(6) . . . . ? N3 Cd1 N1 C1 58.4(6) 7_666 . . . ? O5 Cd1 N1 C1 -43.5(6) . . . . ? O5 Cd1 N1 C1 136.5(6) 7_666 . . . ? N1 Cd1 N1 C5 -45(100) 7_666 . . . ? N3 Cd1 N1 C5 45.8(5) . . . . ? N3 Cd1 N1 C5 -134.2(5) 7_666 . . . ? O5 Cd1 N1 C5 123.9(6) . . . . ? O5 Cd1 N1 C5 -56.1(6) 7_666 . . . ? C5 N1 C1 C2 -0.1(13) . . . . ? Cd1 N1 C1 C2 168.0(7) . . . . ? N1 C1 C2 C3 -1.5(15) . . . . ? C1 C2 C3 C4 0.2(13) . . . . ? C2 C3 C4 C5 2.5(10) . . . . ? C2 C3 C4 C6 -179.5(7) . . . . ? C1 N1 C5 C4 3.1(10) . . . . ? Cd1 N1 C5 C4 -164.5(5) . . . . ? C3 C4 C5 N1 -4.3(10) . . . . ? C6 C4 C5 N1 177.7(6) . . . . ? C5 C4 C6 O1 148.0(7) . . . . ? C3 C4 C6 O1 -29.9(10) . . . . ? C5 C4 C6 C7 -33.1(9) . . . . ? C3 C4 C6 C7 148.9(6) . . . . ? C11 N2 C7 C8 -0.2(9) . . . . ? C11 N2 C7 C6 -175.5(5) . . . . ? O1 C6 C7 N2 158.3(6) . . . . ? C4 C6 C7 N2 -20.6(9) . . . . ? O1 C6 C7 C8 -17.3(9) . . . . ? C4 C6 C7 C8 163.8(6) . . . . ? N2 C7 C8 C9 1.1(10) . . . . ? C6 C7 C8 C9 176.4(6) . . . . ? C7 C8 C9 C10 -1.7(10) . . . . ? C8 C9 C10 C11 1.5(10) . . . . ? C7 N2 C11 C10 0.0(8) . . . . ? C7 N2 C11 C12 176.2(5) . . . . ? C9 C10 C11 N2 -0.7(10) . . . . ? C9 C10 C11 C12 -176.8(6) . . . . ? N2 C11 C12 O2 -156.2(5) . . . . ? C10 C11 C12 O2 20.1(8) . . . . ? N2 C11 C12 C14 23.4(8) . . . . ? C10 C11 C12 C14 -160.3(6) . . . . ? N1 Cd1 N3 C17 123.3(6) . . . . ? N1 Cd1 N3 C17 -56.7(6) 7_666 . . . ? N3 Cd1 N3 C17 -110(100) 7_666 . . . ? O5 Cd1 N3 C17 42.0(6) . . . . ? O5 Cd1 N3 C17 -138.0(6) 7_666 . . . ? N1 Cd1 N3 C13 -41.6(5) . . . . ? N1 Cd1 N3 C13 138.4(5) 7_666 . . . ? N3 Cd1 N3 C13 85(100) 7_666 . . . ? O5 Cd1 N3 C13 -122.9(6) . . . . ? O5 Cd1 N3 C13 57.1(6) 7_666 . . . ? C17 N3 C13 C14 -0.9(10) . . . . ? Cd1 N3 C13 C14 164.4(5) . . . . ? N3 C13 C14 C15 2.3(10) . . . . ? N3 C13 C14 C12 -178.4(6) . . . . ? O2 C12 C14 C13 -154.1(6) . . . . ? C11 C12 C14 C13 26.3(9) . . . . ? O2 C12 C14 C15 25.2(9) . . . . ? C11 C12 C14 C15 -154.4(6) . . . . ? C13 C14 C15 C16 -1.8(12) . . . . ? C12 C14 C15 C16 178.8(8) . . . . ? C14 C15 C16 C17 0.3(14) . . . . ? C13 N3 C17 C16 -0.8(12) . . . . ? Cd1 N3 C17 C16 -166.6(7) . . . . ? C15 C16 C17 N3 1.2(15) . . . . ? O8 Cd2 N4 C22 148.9(7) 5_666 . . . ? O8 Cd2 N4 C22 -31.1(7) . . . . ? N4 Cd2 N4 C22 150(100) 5_666 . . . ? N6 Cd2 N4 C22 -119.6(7) . . . . ? N6 Cd2 N4 C22 60.4(7) 5_666 . . . ? O8 Cd2 N4 C18 -41.8(6) 5_666 . . . ? O8 Cd2 N4 C18 138.2(6) . . . . ? N4 Cd2 N4 C18 -41(100) 5_666 . . . ? N6 Cd2 N4 C18 49.7(6) . . . . ? N6 Cd2 N4 C18 -130.3(6) 5_666 . . . ? C22 N4 C18 C19 2.7(11) . . . . ? Cd2 N4 C18 C19 -166.8(5) . . . . ? N4 C18 C19 C20 -1.8(10) . . . . ? N4 C18 C19 C23 178.7(6) . . . . ? C18 C19 C20 C21 0.4(11) . . . . ? C23 C19 C20 C21 179.9(8) . . . . ? C19 C20 C21 C22 0.1(13) . . . . ? C18 N4 C22 C21 -2.2(13) . . . . ? Cd2 N4 C22 C21 167.5(7) . . . . ? C20 C21 C22 N4 0.8(15) . . . . ? C20 C19 C23 O3 -28.3(10) . . . . ? C18 C19 C23 O3 151.2(7) . . . . ? C20 C19 C23 C24 148.8(7) . . . . ? C18 C19 C23 C24 -31.7(9) . . . . ? C28 N5 C24 C25 -0.5(9) . . . . ? C28 N5 C24 C23 -176.5(5) . . . . ? O3 C23 C24 N5 157.4(7) . . . . ? C19 C23 C24 N5 -19.7(9) . . . . ? O3 C23 C24 C25 -18.8(10) . . . . ? C19 C23 C24 C25 164.1(6) . . . . ? N5 C24 C25 C26 -1.9(10) . . . . ? C23 C24 C25 C26 174.1(6) . . . . ? C24 C25 C26 C27 2.9(11) . . . . ? C24 N5 C28 C27 1.8(9) . . . . ? C24 N5 C28 C29 177.1(5) . . . . ? O8 Cd2 N6 C30 34.1(6) 5_666 . . . ? O8 Cd2 N6 C30 -145.9(6) . . . . ? N4 Cd2 N6 C30 128.6(6) 5_666 . . . ? N4 Cd2 N6 C30 -51.4(6) . . . . ? N6 Cd2 N6 C30 117(100) 5_666 . . . ? O8 Cd2 N6 C34 -160.0(6) 5_666 . . . ? O8 Cd2 N6 C34 20.0(6) . . . . ? N4 Cd2 N6 C34 -65.5(6) 5_666 . . . ? N4 Cd2 N6 C34 114.5(6) . . . . ? N6 Cd2 N6 C34 -77(100) 5_666 . . . ? N5 C28 C29 O4 -164.8(6) . . . . ? C27 C28 C29 O4 10.7(9) . . . . ? N5 C28 C29 C31 13.6(8) . . . . ? C27 C28 C29 C31 -170.9(6) . . . . ? C34 N6 C30 C31 -2.0(11) . . . . ? Cd2 N6 C30 C31 164.4(5) . . . . ? N6 C30 C31 C32 3.4(11) . . . . ? N6 C30 C31 C29 177.9(6) . . . . ? O4 C29 C31 C30 -138.2(8) . . . . ? C28 C29 C31 C30 43.5(9) . . . . ? O4 C29 C31 C32 36.3(10) . . . . ? C28 C29 C31 C32 -142.0(6) . . . . ? C30 C31 C32 C33 -1.5(11) . . . . ? C29 C31 C32 C33 -176.2(7) . . . . ? C31 C32 C33 C34 -1.6(12) . . . . ? C32 C33 C34 N6 3.2(14) . . . . ? C30 N6 C34 C33 -1.4(12) . . . . ? Cd2 N6 C34 C33 -168.1(7) . . . . ? C25 C26 C27 C28 -1.6(11) . . . . ? N5 C28 C27 C26 -0.8(10) . . . . ? C29 C28 C27 C26 -176.1(6) . . . . ? O7 N7 O5 Cd1 170.2(6) . . . . ? O6 N7 O5 Cd1 -6.3(12) . . . . ? N1 Cd1 O5 N7 129.8(8) . . . . ? N1 Cd1 O5 N7 -50.2(8) 7_666 . . . ? N3 Cd1 O5 N7 -134.9(8) . . . . ? N3 Cd1 O5 N7 45.1(8) 7_666 . . . ? O5 Cd1 O5 N7 -165(100) 7_666 . . . ? O10 N8 O8 Cd2 34(3) . . . . ? O9 N8 O8 Cd2 -159.8(13) . . . . ? O8 Cd2 O8 N8 -2(100) 5_666 . . . ? N4 Cd2 O8 N8 -150.7(15) 5_666 . . . ? N4 Cd2 O8 N8 29.3(15) . . . . ? N6 Cd2 O8 N8 119.5(15) . . . . ? N6 Cd2 O8 N8 -60.5(15) 5_666 . . . ? O3W' O3W O3W' O3W 0.000(3) 5_676 . . 5_676 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.888 _refine_diff_density_min -0.726 _refine_diff_density_rms 0.106 ##############################end######################## data_complex3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H26 Cd N8 O12' _chemical_formula_weight 851.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.192(13) _cell_length_b 9.862(6) _cell_length_c 17.081(9) _cell_angle_alpha 90.00 _cell_angle_beta 113.969(10) _cell_angle_gamma 90.00 _cell_volume 3570(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.687 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.871676 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11892 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4396 _reflns_number_gt 3460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELTXL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+7.1568P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4396 _refine_ls_number_parameters 235 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.1003 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.2500 0.2500 0.5000 0.03599(10) Uani 1 2 d S . . N1 N 0.27806(12) 0.4828(2) 0.51837(16) 0.0411(5) Uani 1 1 d . . . N2 N 0.41239(11) 0.5107(3) 0.42258(16) 0.0439(6) Uani 1 1 d . . . N3 N 0.35580(11) 0.1960(3) 0.52813(17) 0.0421(5) Uani 1 1 d . . . C1 C 0.30351(12) 0.5415(3) 0.46908(19) 0.0395(6) Uani 1 1 d . . . H1A H 0.2991 0.4979 0.4187 0.047 Uiso 1 1 calc R . . C2 C 0.33594(13) 0.6631(3) 0.4890(2) 0.0429(6) Uani 1 1 d . . . C3 C 0.34098(18) 0.7290(3) 0.5630(3) 0.0554(8) Uani 1 1 d . . . H3A H 0.3620 0.8116 0.5780 0.067 Uiso 1 1 calc R . . C4 C 0.31479(19) 0.6716(4) 0.6138(2) 0.0604(9) Uani 1 1 d . . . H4A H 0.3176 0.7147 0.6636 0.072 Uiso 1 1 calc R . . C5 C 0.28401(16) 0.5482(3) 0.5898(2) 0.0514(7) Uani 1 1 d . . . H5A H 0.2667 0.5092 0.6250 0.062 Uiso 1 1 calc R . . C6 C 0.36302(15) 0.7241(3) 0.4317(2) 0.0509(8) Uani 1 1 d . . . C7 C 0.39212(13) 0.6327(3) 0.3874(2) 0.0481(7) Uani 1 1 d . . . C8 C 0.39800(18) 0.6775(4) 0.3136(2) 0.0605(9) Uiso 1 1 d . . . H8A H 0.3845 0.7637 0.2918 0.073 Uiso 1 1 calc R . . C9 C 0.4240(2) 0.5919(4) 0.2742(3) 0.0721(10) Uiso 1 1 d . . . H9A H 0.4270 0.6178 0.2236 0.087 Uiso 1 1 calc R . . C10 C 0.44584(19) 0.4664(4) 0.3099(3) 0.0675(10) Uiso 1 1 d . . . H10A H 0.4645 0.4075 0.2845 0.081 Uiso 1 1 calc R . . C11 C 0.43944(14) 0.4298(4) 0.3847(2) 0.0495(7) Uani 1 1 d . . . C12 C 0.46602(15) 0.2960(4) 0.4266(2) 0.0512(7) Uani 1 1 d . . . C13 C 0.39317(15) 0.1126(3) 0.5900(2) 0.0501(7) Uani 1 1 d . . . H13A H 0.3773 0.0734 0.6267 0.060 Uiso 1 1 calc R . . C14 C 0.45416(16) 0.0826(4) 0.6014(2) 0.0566(8) Uani 1 1 d . . . H14A H 0.4785 0.0232 0.6444 0.068 Uiso 1 1 calc R . . C15 C 0.47858(15) 0.1415(3) 0.5483(2) 0.0521(8) Uani 1 1 d . . . H15A H 0.5193 0.1210 0.5543 0.063 Uiso 1 1 calc R . . C16 C 0.44171(15) 0.2314(3) 0.4862(2) 0.0449(7) Uani 1 1 d . . . C17 C 0.38020(14) 0.2539(3) 0.4776(2) 0.0433(6) Uani 1 1 d . . . H17A H 0.3548 0.3121 0.4346 0.052 Uiso 1 1 calc R . . O2 O 0.50784(15) 0.2418(3) 0.4123(2) 0.0762(9) Uani 1 1 d . . . O1 O 0.36265(13) 0.8464(3) 0.4217(2) 0.0753(8) Uani 1 1 d . . . N4 N 0.1939(2) 0.4339(3) 0.7441(2) 0.0753(10) Uani 1 1 d U . . O3 O 0.2458(2) 0.4816(5) 0.7533(2) 0.1315(18) Uani 1 1 d U . . O4 O 0.1768(3) 0.3300(4) 0.7041(2) 0.1341(18) Uani 1 1 d U . . O5 O 0.16474(18) 0.4943(3) 0.7775(2) 0.0920(10) Uani 1 1 d U . . O1W O 0.27020(12) 0.2327(2) 0.64414(14) 0.0513(5) Uani 1 1 d . . . H1WA H 0.2816 0.1505 0.6674 0.077 Uiso 1 1 d R . . H1WB H 0.2479 0.2750 0.6686 0.077 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03497(15) 0.03676(16) 0.04319(16) -0.00212(12) 0.02301(12) -0.00569(11) N1 0.0433(12) 0.0371(12) 0.0512(14) -0.0045(10) 0.0278(11) -0.0034(10) N2 0.0345(11) 0.0488(14) 0.0544(14) 0.0053(12) 0.0244(11) -0.0026(10) N3 0.0392(12) 0.0392(12) 0.0569(15) 0.0004(11) 0.0287(11) -0.0022(10) C1 0.0354(13) 0.0398(14) 0.0467(15) -0.0023(12) 0.0201(12) -0.0038(11) C2 0.0343(13) 0.0376(14) 0.0568(17) 0.0052(13) 0.0185(13) 0.0015(11) C3 0.0552(19) 0.0343(16) 0.074(2) -0.0082(14) 0.0234(17) -0.0030(13) C4 0.078(2) 0.0482(19) 0.058(2) -0.0147(16) 0.0302(18) 0.0016(17) C5 0.066(2) 0.0434(16) 0.0559(18) -0.0004(14) 0.0364(16) 0.0044(15) C6 0.0367(14) 0.0452(18) 0.070(2) 0.0137(15) 0.0205(15) -0.0007(12) C7 0.0321(13) 0.0552(18) 0.0564(18) 0.0116(14) 0.0172(13) -0.0076(13) C11 0.0392(15) 0.062(2) 0.0561(18) 0.0010(15) 0.0285(14) -0.0053(14) C12 0.0416(16) 0.0589(18) 0.065(2) -0.0047(16) 0.0334(15) -0.0036(14) C13 0.0542(18) 0.0417(16) 0.063(2) 0.0036(14) 0.0320(16) -0.0015(14) C14 0.0517(18) 0.0474(18) 0.069(2) 0.0103(16) 0.0232(16) 0.0066(15) C15 0.0412(15) 0.0429(17) 0.076(2) -0.0033(15) 0.0275(16) 0.0025(13) C16 0.0395(14) 0.0424(16) 0.0610(18) -0.0058(13) 0.0288(14) -0.0028(12) C17 0.0386(14) 0.0427(15) 0.0539(16) 0.0018(13) 0.0244(13) 0.0005(12) O2 0.0684(17) 0.081(2) 0.107(2) 0.0052(15) 0.0639(18) 0.0141(14) O1 0.0697(16) 0.0462(14) 0.122(2) 0.0264(15) 0.0515(17) 0.0035(12) N4 0.136(3) 0.0590(19) 0.0482(17) 0.0084(15) 0.055(2) 0.018(2) O3 0.122(3) 0.208(6) 0.080(2) 0.027(3) 0.057(2) 0.013(4) O4 0.262(6) 0.064(2) 0.085(2) -0.0235(19) 0.080(3) -0.005(3) O5 0.133(3) 0.085(2) 0.093(2) -0.0077(17) 0.083(2) 0.012(2) O1W 0.0645(14) 0.0484(13) 0.0439(11) 0.0011(9) 0.0250(11) 0.0013(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1W 2.318(3) . ? Cd1 O1W 2.318(3) 7_556 ? Cd1 N3 2.362(3) 7_556 ? Cd1 N3 2.362(3) . ? Cd1 N1 2.372(3) 7_556 ? Cd1 N1 2.372(3) . ? N1 C5 1.337(4) . ? N1 C1 1.340(3) . ? N2 C11 1.334(4) . ? N2 C7 1.342(4) . ? N3 C17 1.337(4) . ? N3 C13 1.342(4) . ? C1 C2 1.383(4) . ? C1 H1A 0.9300 . ? C2 C3 1.383(5) . ? C2 C6 1.487(4) . ? C3 C4 1.368(5) . ? C3 H3A 0.9300 . ? C4 C5 1.386(5) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 O1 1.218(4) . ? C6 C7 1.502(5) . ? C7 C8 1.393(5) . ? C8 C9 1.363(5) . ? C8 H8A 0.9300 . ? C9 C10 1.383(6) . ? C9 H9A 0.9300 . ? C10 C11 1.391(5) . ? C10 H10A 0.9300 . ? C11 C12 1.509(5) . ? C12 O2 1.215(4) . ? C12 C16 1.492(4) . ? C13 C14 1.379(5) . ? C13 H13A 0.9300 . ? C14 C15 1.377(5) . ? C14 H14A 0.9300 . ? C15 C16 1.381(5) . ? C15 H15A 0.9300 . ? C16 C17 1.391(4) . ? C17 H17A 0.9300 . ? N4 O5 1.204(4) . ? N4 O4 1.206(5) . ? N4 O3 1.242(5) . ? O1W H1WA 0.8943 . ? O1W H1WB 0.8901 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Cd1 O1W 180.0 . 7_556 ? O1W Cd1 N3 88.72(9) . 7_556 ? O1W Cd1 N3 91.28(9) 7_556 7_556 ? O1W Cd1 N3 91.28(9) . . ? O1W Cd1 N3 88.72(9) 7_556 . ? N3 Cd1 N3 180.00(13) 7_556 . ? O1W Cd1 N1 89.75(8) . 7_556 ? O1W Cd1 N1 90.25(8) 7_556 7_556 ? N3 Cd1 N1 89.14(9) 7_556 7_556 ? N3 Cd1 N1 90.86(9) . 7_556 ? O1W Cd1 N1 90.25(8) . . ? O1W Cd1 N1 89.75(8) 7_556 . ? N3 Cd1 N1 90.86(9) 7_556 . ? N3 Cd1 N1 89.14(9) . . ? N1 Cd1 N1 180.000(1) 7_556 . ? C5 N1 C1 117.2(3) . . ? C5 N1 Cd1 120.6(2) . . ? C1 N1 Cd1 120.11(19) . . ? C11 N2 C7 117.8(3) . . ? C17 N3 C13 117.6(3) . . ? C17 N3 Cd1 116.7(2) . . ? C13 N3 Cd1 125.7(2) . . ? N1 C1 C2 123.6(3) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? C3 C2 C1 117.9(3) . . ? C3 C2 C6 120.6(3) . . ? C1 C2 C6 121.4(3) . . ? C4 C3 C2 119.4(3) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 119.0(3) . . ? C3 C4 H4A 120.5 . . ? C5 C4 H4A 120.5 . . ? N1 C5 C4 122.9(3) . . ? N1 C5 H5A 118.6 . . ? C4 C5 H5A 118.6 . . ? O1 C6 C2 120.8(3) . . ? O1 C6 C7 120.1(3) . . ? C2 C6 C7 119.0(3) . . ? N2 C7 C8 123.0(3) . . ? N2 C7 C6 117.3(3) . . ? C8 C7 C6 119.7(3) . . ? C9 C8 C7 118.4(4) . . ? C9 C8 H8A 120.8 . . ? C7 C8 H8A 120.8 . . ? C8 C9 C10 119.5(4) . . ? C8 C9 H9A 120.3 . . ? C10 C9 H9A 120.3 . . ? C9 C10 C11 118.7(4) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? N2 C11 C10 122.5(3) . . ? N2 C11 C12 118.3(3) . . ? C10 C11 C12 119.1(3) . . ? O2 C12 C16 120.2(3) . . ? O2 C12 C11 119.6(3) . . ? C16 C12 C11 120.2(3) . . ? N3 C13 C14 122.6(3) . . ? N3 C13 H13A 118.7 . . ? C14 C13 H13A 118.7 . . ? C15 C14 C13 119.3(3) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C14 C15 C16 119.0(3) . . ? C14 C15 H15A 120.5 . . ? C16 C15 H15A 120.5 . . ? C15 C16 C17 118.1(3) . . ? C15 C16 C12 120.7(3) . . ? C17 C16 C12 121.0(3) . . ? N3 C17 C16 123.3(3) . . ? N3 C17 H17A 118.4 . . ? C16 C17 H17A 118.4 . . ? O5 N4 O4 124.7(5) . . ? O5 N4 O3 117.1(4) . . ? O4 N4 O3 118.2(5) . . ? Cd1 O1W H1WA 115.7 . . ? Cd1 O1W H1WB 124.0 . . ? H1WA O1W H1WB 109.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1W Cd1 N1 C5 -13.3(2) . . . . ? O1W Cd1 N1 C5 166.7(2) 7_556 . . . ? N3 Cd1 N1 C5 75.4(2) 7_556 . . . ? N3 Cd1 N1 C5 -104.6(2) . . . . ? N1 Cd1 N1 C5 -136(100) 7_556 . . . ? O1W Cd1 N1 C1 149.6(2) . . . . ? O1W Cd1 N1 C1 -30.4(2) 7_556 . . . ? N3 Cd1 N1 C1 -121.6(2) 7_556 . . . ? N3 Cd1 N1 C1 58.4(2) . . . . ? N1 Cd1 N1 C1 27(100) 7_556 . . . ? O1W Cd1 N3 C17 -147.2(2) . . . . ? O1W Cd1 N3 C17 32.8(2) 7_556 . . . ? N3 Cd1 N3 C17 17(36) 7_556 . . . ? N1 Cd1 N3 C17 123.0(2) 7_556 . . . ? N1 Cd1 N3 C17 -57.0(2) . . . . ? O1W Cd1 N3 C13 32.9(3) . . . . ? O1W Cd1 N3 C13 -147.1(3) 7_556 . . . ? N3 Cd1 N3 C13 -163(36) 7_556 . . . ? N1 Cd1 N3 C13 -56.9(3) 7_556 . . . ? N1 Cd1 N3 C13 123.1(3) . . . . ? C5 N1 C1 C2 1.1(4) . . . . ? Cd1 N1 C1 C2 -162.5(2) . . . . ? N1 C1 C2 C3 -1.5(4) . . . . ? N1 C1 C2 C6 -179.7(3) . . . . ? C1 C2 C3 C4 0.8(5) . . . . ? C6 C2 C3 C4 179.0(3) . . . . ? C2 C3 C4 C5 0.2(5) . . . . ? C1 N1 C5 C4 0.1(5) . . . . ? Cd1 N1 C5 C4 163.6(3) . . . . ? C3 C4 C5 N1 -0.7(6) . . . . ? C3 C2 C6 O1 -35.1(5) . . . . ? C1 C2 C6 O1 143.0(3) . . . . ? C3 C2 C6 C7 143.8(3) . . . . ? C1 C2 C6 C7 -38.1(4) . . . . ? C11 N2 C7 C8 0.2(4) . . . . ? C11 N2 C7 C6 -178.7(3) . . . . ? O1 C6 C7 N2 156.0(3) . . . . ? C2 C6 C7 N2 -22.9(4) . . . . ? O1 C6 C7 C8 -22.9(5) . . . . ? C2 C6 C7 C8 158.2(3) . . . . ? N2 C7 C8 C9 1.8(5) . . . . ? C6 C7 C8 C9 -179.3(3) . . . . ? C7 C8 C9 C10 -2.5(6) . . . . ? C8 C9 C10 C11 1.3(6) . . . . ? C7 N2 C11 C10 -1.5(5) . . . . ? C7 N2 C11 C12 176.3(3) . . . . ? C9 C10 C11 N2 0.8(6) . . . . ? C9 C10 C11 C12 -177.0(3) . . . . ? N2 C11 C12 O2 -155.5(3) . . . . ? C10 C11 C12 O2 22.3(5) . . . . ? N2 C11 C12 C16 23.6(5) . . . . ? C10 C11 C12 C16 -158.5(3) . . . . ? C17 N3 C13 C14 -1.7(5) . . . . ? Cd1 N3 C13 C14 178.2(3) . . . . ? N3 C13 C14 C15 1.0(5) . . . . ? C13 C14 C15 C16 1.3(5) . . . . ? C14 C15 C16 C17 -2.7(5) . . . . ? C14 C15 C16 C12 -179.1(3) . . . . ? O2 C12 C16 C15 23.7(5) . . . . ? C11 C12 C16 C15 -155.4(3) . . . . ? O2 C12 C16 C17 -152.6(4) . . . . ? C11 C12 C16 C17 28.3(5) . . . . ? C13 N3 C17 C16 0.2(5) . . . . ? Cd1 N3 C17 C16 -179.7(2) . . . . ? C15 C16 C17 N3 2.1(5) . . . . ? C12 C16 C17 N3 178.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.682 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.072 ############################end########################### data_complex4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H28 Cd Cl2 N6 O15' _chemical_formula_weight 943.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0026(8) _cell_length_b 12.8675(10) _cell_length_c 15.4829(12) _cell_angle_alpha 80.627(2) _cell_angle_beta 71.799(2) _cell_angle_gamma 84.189(2) _cell_volume 1865.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.810 _exptl_absorpt_correction_type Multi-SCAN _exptl_absorpt_correction_T_min 0.807380 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27091 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6568 _reflns_number_gt 5252 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker 2007)' _computing_cell_refinement 'APEX2 and SAINT (Bruker 2007)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+3.0657P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6568 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1227 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.5000 1.0000 0.03808(13) Uani 1 2 d S . . Cd2 Cd 0.5000 0.5000 0.5000 0.04175(13) Uani 1 2 d S . . O1 O -0.1429(3) 0.7384(3) 1.0041(3) 0.0715(10) Uani 1 1 d . . . O2 O 0.4034(4) 1.0392(2) 0.9374(3) 0.0655(9) Uani 1 1 d . . . O3 O 0.0912(5) 0.8846(4) 0.7178(3) 0.1025(15) Uani 1 1 d . . . O4 O 0.5917(6) 1.0080(3) 0.2945(3) 0.1130(18) Uani 1 1 d . . . N1 N 0.2799(3) 0.5294(2) 0.9684(3) 0.0452(8) Uani 1 1 d . . . N2 N 0.1737(3) 0.8400(2) 0.9896(2) 0.0420(8) Uani 1 1 d . . . N3 N 0.5564(3) 0.6776(2) 0.9440(2) 0.0399(7) Uani 1 1 d . . . N4 N 0.4031(4) 0.6040(3) 0.6180(2) 0.0460(8) Uani 1 1 d . . . N5 N 0.3537(5) 0.9029(3) 0.5034(3) 0.0622(11) Uani 1 1 d . . . N6 N 0.6097(4) 0.6482(3) 0.4097(3) 0.0550(9) Uani 1 1 d . . . C1 C 0.2579(5) 0.4831(3) 0.9028(3) 0.0534(11) Uani 1 1 d . . . H1A H 0.3192 0.4274 0.8809 0.064 Uiso 1 1 calc R . . C2 C 0.1485(5) 0.5145(4) 0.8663(4) 0.0580(12) Uani 1 1 d . . . H2A H 0.1353 0.4791 0.8220 0.070 Uiso 1 1 calc R . . C3 C 0.0591(4) 0.5984(4) 0.8960(3) 0.0543(11) Uani 1 1 d . . . H3A H -0.0132 0.6222 0.8706 0.065 Uiso 1 1 calc R . . C4 C 0.0786(4) 0.6468(3) 0.9641(3) 0.0447(9) Uani 1 1 d . . . C5 C 0.1897(4) 0.6093(3) 0.9990(3) 0.0430(9) Uani 1 1 d . . . H5A H 0.2018 0.6410 1.0456 0.052 Uiso 1 1 calc R . . C6 C -0.0193(4) 0.7351(3) 1.0006(3) 0.0499(10) Uani 1 1 d . . . C7 C 0.0368(4) 0.8214(3) 1.0318(3) 0.0454(9) Uani 1 1 d . . . C8 C -0.0506(5) 0.8809(4) 1.0961(3) 0.0535(11) Uani 1 1 d . . . H8A H -0.1446 0.8657 1.1237 0.064 Uiso 1 1 calc R . . C9 C 0.0036(5) 0.9628(4) 1.1187(3) 0.0576(12) Uani 1 1 d . . . H9A H -0.0522 1.0024 1.1634 0.069 Uiso 1 1 calc R . . C10 C 0.1420(5) 0.9855(3) 1.0742(3) 0.0528(11) Uani 1 1 d . . . H10A H 0.1806 1.0419 1.0869 0.063 Uiso 1 1 calc R . . C11 C 0.2230(4) 0.9224(3) 1.0099(3) 0.0428(9) Uani 1 1 d . . . C12 C 0.3724(5) 0.9479(3) 0.9566(3) 0.0462(10) Uani 1 1 d . . . C13 C 0.4794(4) 0.8608(3) 0.9264(3) 0.0399(9) Uani 1 1 d . . . C14 C 0.6027(5) 0.8831(3) 0.8556(3) 0.0490(10) Uani 1 1 d . . . H14A H 0.6180 0.9514 0.8253 0.059 Uiso 1 1 calc R . . C15 C 0.7022(5) 0.8019(4) 0.8309(3) 0.0518(10) Uani 1 1 d . . . H15A H 0.7867 0.8149 0.7847 0.062 Uiso 1 1 calc R . . C16 C 0.6742(4) 0.7016(3) 0.8757(3) 0.0441(9) Uani 1 1 d . . . H16A H 0.7409 0.6473 0.8575 0.053 Uiso 1 1 calc R . . C17 C 0.4624(4) 0.7573(3) 0.9690(3) 0.0409(9) Uani 1 1 d . . . H17A H 0.3812 0.7425 1.0176 0.049 Uiso 1 1 calc R . . C18 C 0.4630(5) 0.5952(4) 0.6859(3) 0.0567(11) Uani 1 1 d . . . H18A H 0.5272 0.5388 0.6909 0.068 Uiso 1 1 calc R . . C19 C 0.4337(6) 0.6652(4) 0.7473(3) 0.0633(13) Uani 1 1 d . . . H19A H 0.4751 0.6552 0.7943 0.076 Uiso 1 1 calc R . . C20 C 0.3412(5) 0.7517(4) 0.7391(3) 0.0600(12) Uani 1 1 d . . . H20A H 0.3193 0.8003 0.7805 0.072 Uiso 1 1 calc R . . C21 C 0.2831(5) 0.7636(3) 0.6687(3) 0.0501(10) Uani 1 1 d . . . C22 C 0.3147(4) 0.6872(3) 0.6106(3) 0.0468(10) Uani 1 1 d . . . H22A H 0.2722 0.6944 0.5643 0.056 Uiso 1 1 calc R . . C23 C 0.1889(6) 0.8587(4) 0.6548(4) 0.0682(14) Uani 1 1 d . . . C24 C 0.2302(7) 0.9271(4) 0.5635(4) 0.0715(15) Uani 1 1 d . . . C25 C 0.1448(9) 1.0157(5) 0.5449(6) 0.100(2) Uani 1 1 d . . . H25A H 0.0576 1.0298 0.5866 0.120 Uiso 1 1 calc R . . C26 C 0.1935(12) 1.0816(6) 0.4629(7) 0.128(4) Uani 1 1 d . . . H26A H 0.1400 1.1419 0.4493 0.154 Uiso 1 1 calc R . . C27 C 0.3193(12) 1.0579(5) 0.4026(6) 0.111(3) Uani 1 1 d . . . H27A H 0.3534 1.1020 0.3474 0.133 Uiso 1 1 calc R . . C28 C 0.3975(8) 0.9665(4) 0.4241(4) 0.0775(18) Uani 1 1 d . . . C29 C 0.5363(8) 0.9408(4) 0.3573(4) 0.0764(17) Uani 1 1 d . . . C30 C 0.6115(6) 0.8348(4) 0.3664(3) 0.0613(13) Uani 1 1 d . . . C31 C 0.7584(7) 0.8260(5) 0.3318(4) 0.0841(19) Uani 1 1 d . . . H31A H 0.8090 0.8861 0.3063 0.101 Uiso 1 1 calc R . . C32 C 0.8262(7) 0.7304(6) 0.3354(5) 0.095(2) Uani 1 1 d . . . H32A H 0.9238 0.7237 0.3116 0.114 Uiso 1 1 calc R . . C33 C 0.7495(6) 0.6423(5) 0.3748(4) 0.0792(16) Uani 1 1 d . . . H33A H 0.7972 0.5765 0.3771 0.095 Uiso 1 1 calc R . . C34 C 0.5419(5) 0.7427(3) 0.4046(3) 0.0529(11) Uani 1 1 d . . . H34A H 0.4441 0.7469 0.4277 0.064 Uiso 1 1 calc R . . Cl1 Cl 0.91307(14) 0.58341(15) 0.66657(13) 0.0871(5) Uani 1 1 d . . . O5 O 0.9866(9) 0.5309(6) 0.5961(5) 0.188(3) Uani 1 1 d . . . O6 O 0.9663(9) 0.6707(8) 0.6763(6) 0.220(4) Uani 1 1 d . . . O7 O 0.8965(11) 0.5102(7) 0.7536(5) 0.190(3) Uani 1 1 d . . . O8 O 0.7810(7) 0.6063(9) 0.6661(7) 0.229(5) Uani 1 1 d . . . Cl2 Cl 0.77411(17) 0.19588(14) 0.70434(15) 0.0965(5) Uani 1 1 d . . . O9 O 0.6524(5) 0.1375(4) 0.7376(4) 0.1196(19) Uani 1 1 d . . . O10 O 0.7945(9) 0.2447(7) 0.7737(7) 0.202(4) Uani 1 1 d . . . O11 O 0.8147(11) 0.2227(9) 0.6070(6) 0.126(4) Uani 0.50 1 d P . . O11' O 0.7066(15) 0.3052(8) 0.6941(8) 0.133(4) Uani 0.50 1 d P . . O12 O 0.8868(9) 0.1229(9) 0.7024(7) 0.237(5) Uani 1 1 d . . . O1W O 0.6038(4) 0.4409(3) 0.8577(2) 0.0628(8) Uani 1 1 d . . . O2W O 0.7031(4) 0.4493(3) 0.5497(3) 0.0695(9) Uani 1 1 d . . . O3W O 0.4374(5) 0.2690(3) 0.8477(3) 0.0911(13) Uani 1 1 d . . . H1WA H 0.6868 0.4667 0.8233 0.137 Uiso 1 1 d R . . H1WB H 0.5992 0.3874 0.8302 0.137 Uiso 1 1 d R . . H2WA H 0.7123 0.3904 0.5871 0.137 Uiso 1 1 d R . . H2WB H 0.7411 0.4937 0.5746 0.137 Uiso 1 1 d R . . H3WA H 0.4978 0.2218 0.8176 0.137 Uiso 1 1 d R . . H3WB H 0.3544 0.2366 0.8392 0.137 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0368(2) 0.0261(2) 0.0521(3) -0.00482(16) -0.01691(18) 0.00468(15) Cd2 0.0418(2) 0.0337(2) 0.0511(3) -0.00504(17) -0.01665(19) -0.00112(16) O1 0.0404(17) 0.0534(19) 0.128(3) -0.0191(19) -0.0353(19) 0.0063(14) O2 0.067(2) 0.0270(15) 0.106(3) -0.0060(16) -0.0312(19) -0.0037(14) O3 0.100(3) 0.100(3) 0.103(3) -0.056(3) -0.015(3) 0.034(3) O4 0.194(5) 0.057(2) 0.089(3) 0.024(2) -0.047(3) -0.052(3) N1 0.0403(18) 0.0312(16) 0.068(2) -0.0066(15) -0.0225(17) -0.0004(13) N2 0.0398(18) 0.0298(16) 0.060(2) -0.0080(14) -0.0221(16) 0.0067(13) N3 0.0376(17) 0.0308(16) 0.056(2) -0.0066(14) -0.0221(16) 0.0026(13) N4 0.050(2) 0.0420(18) 0.049(2) -0.0039(15) -0.0185(16) -0.0054(15) N5 0.092(3) 0.040(2) 0.066(3) -0.0118(19) -0.042(2) 0.007(2) N6 0.049(2) 0.048(2) 0.062(2) -0.0055(17) -0.0060(18) -0.0079(17) C1 0.044(2) 0.042(2) 0.076(3) -0.016(2) -0.016(2) -0.0048(18) C2 0.049(3) 0.060(3) 0.072(3) -0.020(2) -0.021(2) -0.010(2) C3 0.041(2) 0.053(3) 0.076(3) -0.004(2) -0.028(2) -0.0071(19) C4 0.036(2) 0.034(2) 0.067(3) -0.0036(18) -0.0211(19) -0.0032(16) C5 0.039(2) 0.0294(19) 0.065(3) -0.0061(17) -0.0214(19) -0.0023(16) C6 0.037(2) 0.038(2) 0.075(3) 0.001(2) -0.023(2) 0.0009(17) C7 0.043(2) 0.036(2) 0.059(3) -0.0032(18) -0.0226(19) 0.0070(17) C8 0.050(2) 0.051(3) 0.055(3) 0.000(2) -0.015(2) 0.007(2) C9 0.068(3) 0.053(3) 0.049(3) -0.010(2) -0.018(2) 0.013(2) C10 0.070(3) 0.038(2) 0.059(3) -0.0138(19) -0.031(2) 0.009(2) C11 0.048(2) 0.0283(19) 0.058(3) -0.0067(17) -0.026(2) 0.0063(16) C12 0.051(2) 0.031(2) 0.066(3) -0.0057(18) -0.031(2) 0.0009(17) C13 0.042(2) 0.0289(18) 0.056(2) -0.0058(17) -0.0247(19) -0.0019(15) C14 0.055(3) 0.037(2) 0.059(3) -0.0002(19) -0.025(2) -0.0085(18) C15 0.044(2) 0.054(3) 0.056(3) -0.006(2) -0.013(2) -0.0077(19) C16 0.038(2) 0.042(2) 0.055(3) -0.0119(19) -0.0185(19) 0.0037(17) C17 0.038(2) 0.034(2) 0.054(2) -0.0051(17) -0.0208(18) -0.0009(16) C18 0.065(3) 0.055(3) 0.054(3) 0.001(2) -0.028(2) -0.005(2) C19 0.078(3) 0.068(3) 0.052(3) 0.000(2) -0.032(3) -0.017(3) C20 0.073(3) 0.061(3) 0.047(3) -0.010(2) -0.011(2) -0.027(3) C21 0.051(2) 0.049(2) 0.051(3) -0.0126(19) -0.012(2) -0.0073(19) C22 0.045(2) 0.049(2) 0.051(2) -0.0106(19) -0.0196(19) 0.0002(18) C23 0.074(3) 0.062(3) 0.081(4) -0.037(3) -0.032(3) 0.014(3) C24 0.098(4) 0.054(3) 0.083(4) -0.032(3) -0.053(3) 0.024(3) C25 0.129(6) 0.078(4) 0.120(6) -0.046(4) -0.078(5) 0.048(4) C26 0.216(10) 0.070(4) 0.138(7) -0.033(5) -0.122(8) 0.060(6) C27 0.209(10) 0.050(3) 0.102(5) -0.006(3) -0.097(6) 0.018(5) C28 0.143(6) 0.036(3) 0.074(4) -0.007(2) -0.064(4) -0.001(3) C29 0.132(5) 0.045(3) 0.064(3) 0.003(3) -0.046(4) -0.028(3) C30 0.091(4) 0.048(3) 0.046(3) 0.000(2) -0.019(3) -0.026(2) C31 0.097(5) 0.082(4) 0.064(3) -0.007(3) 0.001(3) -0.052(4) C32 0.062(4) 0.101(5) 0.104(5) -0.020(4) 0.012(3) -0.030(3) C33 0.058(3) 0.077(4) 0.087(4) -0.009(3) 0.000(3) -0.007(3) C34 0.060(3) 0.042(2) 0.055(3) -0.0015(19) -0.016(2) -0.011(2) Cl1 0.0499(7) 0.1164(13) 0.1049(12) -0.0599(10) -0.0169(7) 0.0019(7) O5 0.199(7) 0.196(7) 0.124(5) -0.073(5) 0.022(5) 0.047(6) O6 0.175(7) 0.273(10) 0.226(9) -0.101(8) -0.014(6) -0.128(7) O7 0.268(11) 0.179(7) 0.128(6) -0.023(5) -0.068(6) -0.006(7) O8 0.081(4) 0.346(13) 0.302(11) -0.150(10) -0.084(6) 0.046(6) Cl2 0.0639(9) 0.0832(11) 0.1365(16) 0.0170(10) -0.0356(9) -0.0123(8) O9 0.097(3) 0.079(3) 0.160(5) -0.032(3) 0.010(3) -0.034(3) O10 0.177(8) 0.161(7) 0.232(10) -0.076(7) 0.025(7) -0.041(6) O11 0.122(8) 0.152(10) 0.075(6) 0.061(6) -0.009(5) -0.059(7) O11' 0.213(13) 0.080(6) 0.123(9) 0.044(6) -0.098(9) -0.031(7) O12 0.128(6) 0.324(13) 0.250(10) -0.061(9) -0.066(6) 0.093(7) O1W 0.067(2) 0.0581(19) 0.063(2) -0.0213(16) -0.0170(17) 0.0063(16) O2W 0.061(2) 0.066(2) 0.095(3) -0.0084(19) -0.045(2) -0.0012(17) O3W 0.095(3) 0.064(2) 0.107(3) -0.031(2) -0.015(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1W 2.338(3) . ? Cd1 O1W 2.338(3) 2_667 ? Cd1 N3 2.367(3) . ? Cd1 N3 2.367(3) 2_667 ? Cd1 N1 2.382(3) . ? Cd1 N1 2.382(3) 2_667 ? Cd2 N6 2.322(4) 2_666 ? Cd2 N6 2.322(4) . ? Cd2 N4 2.344(4) 2_666 ? Cd2 N4 2.344(4) . ? Cd2 O2W 2.385(3) 2_666 ? Cd2 O2W 2.385(3) . ? O1 C6 1.218(5) . ? O2 C12 1.211(5) . ? O3 C23 1.210(6) . ? O4 C29 1.220(6) . ? N1 C1 1.340(6) . ? N1 C5 1.342(5) . ? N2 C11 1.334(5) . ? N2 C7 1.347(5) . ? N3 C16 1.338(5) . ? N3 C17 1.339(5) . ? N4 C22 1.331(5) . ? N4 C18 1.348(6) . ? N5 C28 1.334(7) . ? N5 C24 1.336(7) . ? N6 C33 1.332(6) . ? N6 C34 1.334(6) . ? C1 C2 1.380(7) . ? C1 H1A 0.9300 . ? C2 C3 1.373(7) . ? C2 H2A 0.9300 . ? C3 C4 1.381(6) . ? C3 H3A 0.9300 . ? C4 C5 1.393(5) . ? C4 C6 1.486(6) . ? C5 H5A 0.9300 . ? C6 C7 1.500(6) . ? C7 C8 1.383(6) . ? C8 C9 1.372(7) . ? C8 H8A 0.9300 . ? C9 C10 1.377(7) . ? C9 H9A 0.9300 . ? C10 C11 1.390(6) . ? C10 H10A 0.9300 . ? C11 C12 1.504(6) . ? C12 C13 1.495(5) . ? C13 C17 1.389(5) . ? C13 C14 1.389(6) . ? C14 C15 1.382(6) . ? C14 H14A 0.9300 . ? C15 C16 1.372(6) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.362(7) . ? C18 H18A 0.9300 . ? C19 C20 1.388(7) . ? C19 H19A 0.9300 . ? C20 C21 1.368(7) . ? C20 H20A 0.9300 . ? C21 C22 1.386(6) . ? C21 C23 1.496(7) . ? C22 H22A 0.9300 . ? C23 C24 1.500(8) . ? C24 C25 1.401(8) . ? C25 C26 1.384(12) . ? C25 H25A 0.9300 . ? C26 C27 1.352(12) . ? C26 H26A 0.9300 . ? C27 C28 1.399(9) . ? C27 H27A 0.9300 . ? C28 C29 1.492(9) . ? C29 C30 1.497(8) . ? C30 C34 1.386(6) . ? C30 C31 1.397(9) . ? C31 C32 1.345(9) . ? C31 H31A 0.9300 . ? C32 C33 1.379(8) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? Cl1 O8 1.326(6) . ? Cl1 O6 1.340(7) . ? Cl1 O5 1.352(6) . ? Cl1 O7 1.486(8) . ? Cl2 O12 1.389(8) . ? Cl2 O10 1.404(10) . ? Cl2 O9 1.407(5) . ? Cl2 O11 1.426(9) . ? Cl2 O11' 1.503(11) . ? O10 O11' 1.767(14) . ? O1W H1WA 0.8976 . ? O1W H1WB 0.8789 . ? O2W H2WA 0.8915 . ? O2W H2WB 0.9099 . ? O3W H3WA 0.8899 . ? O3W H3WB 1.0182 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Cd1 O1W 180.000(1) . 2_667 ? O1W Cd1 N3 94.42(12) . . ? O1W Cd1 N3 85.58(12) 2_667 . ? O1W Cd1 N3 85.58(12) . 2_667 ? O1W Cd1 N3 94.42(12) 2_667 2_667 ? N3 Cd1 N3 180.000(1) . 2_667 ? O1W Cd1 N1 90.03(12) . . ? O1W Cd1 N1 89.97(12) 2_667 . ? N3 Cd1 N1 91.71(11) . . ? N3 Cd1 N1 88.29(11) 2_667 . ? O1W Cd1 N1 89.97(12) . 2_667 ? O1W Cd1 N1 90.03(12) 2_667 2_667 ? N3 Cd1 N1 88.29(11) . 2_667 ? N3 Cd1 N1 91.71(11) 2_667 2_667 ? N1 Cd1 N1 180.000(1) . 2_667 ? N6 Cd2 N6 180.00(12) 2_666 . ? N6 Cd2 N4 87.83(13) 2_666 2_666 ? N6 Cd2 N4 92.17(13) . 2_666 ? N6 Cd2 N4 92.17(13) 2_666 . ? N6 Cd2 N4 87.83(13) . . ? N4 Cd2 N4 180.000(1) 2_666 . ? N6 Cd2 O2W 90.09(13) 2_666 2_666 ? N6 Cd2 O2W 89.91(13) . 2_666 ? N4 Cd2 O2W 92.03(13) 2_666 2_666 ? N4 Cd2 O2W 87.97(13) . 2_666 ? N6 Cd2 O2W 89.91(13) 2_666 . ? N6 Cd2 O2W 90.09(13) . . ? N4 Cd2 O2W 87.97(13) 2_666 . ? N4 Cd2 O2W 92.03(13) . . ? O2W Cd2 O2W 180.00(17) 2_666 . ? C1 N1 C5 117.3(4) . . ? C1 N1 Cd1 120.0(3) . . ? C5 N1 Cd1 120.8(3) . . ? C11 N2 C7 117.0(3) . . ? C16 N3 C17 116.9(3) . . ? C16 N3 Cd1 121.1(3) . . ? C17 N3 Cd1 121.2(3) . . ? C22 N4 C18 117.3(4) . . ? C22 N4 Cd2 122.6(3) . . ? C18 N4 Cd2 118.3(3) . . ? C28 N5 C24 118.7(5) . . ? C33 N6 C34 118.4(4) . . ? C33 N6 Cd2 118.2(4) . . ? C34 N6 Cd2 122.3(3) . . ? N1 C1 C2 122.9(4) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C3 C2 C1 119.4(4) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C2 C3 C4 118.8(4) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C3 C4 C5 118.5(4) . . ? C3 C4 C6 120.4(4) . . ? C5 C4 C6 121.1(4) . . ? N1 C5 C4 123.0(4) . . ? N1 C5 H5A 118.5 . . ? C4 C5 H5A 118.5 . . ? O1 C6 C4 120.7(4) . . ? O1 C6 C7 120.3(4) . . ? C4 C6 C7 119.1(3) . . ? N2 C7 C8 123.1(4) . . ? N2 C7 C6 115.7(4) . . ? C8 C7 C6 121.0(4) . . ? C9 C8 C7 119.0(4) . . ? C9 C8 H8A 120.5 . . ? C7 C8 H8A 120.5 . . ? C8 C9 C10 118.9(4) . . ? C8 C9 H9A 120.6 . . ? C10 C9 H9A 120.6 . . ? C9 C10 C11 118.8(4) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? N2 C11 C10 123.2(4) . . ? N2 C11 C12 116.5(4) . . ? C10 C11 C12 120.2(4) . . ? O2 C12 C13 121.0(4) . . ? O2 C12 C11 119.2(4) . . ? C13 C12 C11 119.7(3) . . ? C17 C13 C14 118.0(4) . . ? C17 C13 C12 122.1(4) . . ? C14 C13 C12 119.9(4) . . ? C15 C14 C13 118.8(4) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? C16 C15 C14 118.8(4) . . ? C16 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? N3 C16 C15 123.8(4) . . ? N3 C16 H16A 118.1 . . ? C15 C16 H16A 118.1 . . ? N3 C17 C13 123.6(4) . . ? N3 C17 H17A 118.2 . . ? C13 C17 H17A 118.2 . . ? N4 C18 C19 122.9(5) . . ? N4 C18 H18A 118.5 . . ? C19 C18 H18A 118.5 . . ? C18 C19 C20 119.3(4) . . ? C18 C19 H19A 120.3 . . ? C20 C19 H19A 120.3 . . ? C21 C20 C19 118.4(4) . . ? C21 C20 H20A 120.8 . . ? C19 C20 H20A 120.8 . . ? C20 C21 C22 118.9(4) . . ? C20 C21 C23 119.9(4) . . ? C22 C21 C23 121.2(4) . . ? N4 C22 C21 123.1(4) . . ? N4 C22 H22A 118.4 . . ? C21 C22 H22A 118.4 . . ? O3 C23 C21 120.9(5) . . ? O3 C23 C24 121.3(5) . . ? C21 C23 C24 117.5(5) . . ? N5 C24 C25 122.1(6) . . ? N5 C24 C23 117.4(4) . . ? C25 C24 C23 120.5(6) . . ? C26 C25 C24 118.3(8) . . ? C26 C25 H25A 120.9 . . ? C24 C25 H25A 120.9 . . ? C27 C26 C25 119.7(7) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 119.2(8) . . ? C26 C27 H27A 120.4 . . ? C28 C27 H27A 120.4 . . ? N5 C28 C27 122.1(7) . . ? N5 C28 C29 118.9(5) . . ? C27 C28 C29 119.0(6) . . ? O4 C29 C28 119.6(6) . . ? O4 C29 C30 118.7(6) . . ? C28 C29 C30 121.7(5) . . ? C34 C30 C31 117.5(5) . . ? C34 C30 C29 123.1(5) . . ? C31 C30 C29 119.4(5) . . ? C32 C31 C30 119.8(5) . . ? C32 C31 H31A 120.1 . . ? C30 C31 H31A 120.1 . . ? C31 C32 C33 119.3(6) . . ? C31 C32 H32A 120.3 . . ? C33 C32 H32A 120.3 . . ? N6 C33 C32 122.4(6) . . ? N6 C33 H33A 118.8 . . ? C32 C33 H33A 118.8 . . ? N6 C34 C30 122.6(5) . . ? N6 C34 H34A 118.7 . . ? C30 C34 H34A 118.7 . . ? O8 Cl1 O6 108.6(7) . . ? O8 Cl1 O5 111.4(6) . . ? O6 Cl1 O5 117.9(5) . . ? O8 Cl1 O7 102.8(6) . . ? O6 Cl1 O7 106.8(6) . . ? O5 Cl1 O7 108.2(5) . . ? O12 Cl2 O10 93.8(6) . . ? O12 Cl2 O9 105.9(6) . . ? O10 Cl2 O9 111.2(4) . . ? O12 Cl2 O11 93.7(7) . . ? O10 Cl2 O11 132.0(6) . . ? O9 Cl2 O11 112.0(5) . . ? O12 Cl2 O11' 154.5(7) . . ? O10 Cl2 O11' 74.8(6) . . ? O9 Cl2 O11' 99.5(6) . . ? O11 Cl2 O11' 78.5(7) . . ? Cl2 O10 O11' 55.2(6) . . ? Cl2 O11' O10 50.1(4) . . ? Cd1 O1W H1WA 117.1 . . ? Cd1 O1W H1WB 138.6 . . ? H1WA O1W H1WB 102.1 . . ? Cd2 O2W H2WA 124.3 . . ? Cd2 O2W H2WB 122.2 . . ? H2WA O2W H2WB 98.0 . . ? H3WA O3W H3WB 91.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1W Cd1 N1 C1 18.1(3) . . . . ? O1W Cd1 N1 C1 -161.9(3) 2_667 . . . ? N3 Cd1 N1 C1 112.6(3) . . . . ? N3 Cd1 N1 C1 -67.4(3) 2_667 . . . ? N1 Cd1 N1 C1 -146(100) 2_667 . . . ? O1W Cd1 N1 C5 -146.2(3) . . . . ? O1W Cd1 N1 C5 33.8(3) 2_667 . . . ? N3 Cd1 N1 C5 -51.8(3) . . . . ? N3 Cd1 N1 C5 128.2(3) 2_667 . . . ? N1 Cd1 N1 C5 50(100) 2_667 . . . ? O1W Cd1 N3 C16 -32.6(3) . . . . ? O1W Cd1 N3 C16 147.4(3) 2_667 . . . ? N3 Cd1 N3 C16 45(100) 2_667 . . . ? N1 Cd1 N3 C16 -122.7(3) . . . . ? N1 Cd1 N3 C16 57.3(3) 2_667 . . . ? O1W Cd1 N3 C17 136.8(3) . . . . ? O1W Cd1 N3 C17 -43.2(3) 2_667 . . . ? N3 Cd1 N3 C17 -146(100) 2_667 . . . ? N1 Cd1 N3 C17 46.6(3) . . . . ? N1 Cd1 N3 C17 -133.4(3) 2_667 . . . ? N6 Cd2 N4 C22 -117.1(3) 2_666 . . . ? N6 Cd2 N4 C22 62.9(3) . . . . ? N4 Cd2 N4 C22 178(100) 2_666 . . . ? O2W Cd2 N4 C22 -27.1(3) 2_666 . . . ? O2W Cd2 N4 C22 152.9(3) . . . . ? N6 Cd2 N4 C18 78.9(3) 2_666 . . . ? N6 Cd2 N4 C18 -101.1(3) . . . . ? N4 Cd2 N4 C18 14(100) 2_666 . . . ? O2W Cd2 N4 C18 168.9(3) 2_666 . . . ? O2W Cd2 N4 C18 -11.1(3) . . . . ? N6 Cd2 N6 C33 -155(100) 2_666 . . . ? N4 Cd2 N6 C33 -57.5(4) 2_666 . . . ? N4 Cd2 N6 C33 122.5(4) . . . . ? O2W Cd2 N6 C33 -149.5(4) 2_666 . . . ? O2W Cd2 N6 C33 30.5(4) . . . . ? N6 Cd2 N6 C34 37(100) 2_666 . . . ? N4 Cd2 N6 C34 134.5(4) 2_666 . . . ? N4 Cd2 N6 C34 -45.5(4) . . . . ? O2W Cd2 N6 C34 42.4(4) 2_666 . . . ? O2W Cd2 N6 C34 -137.6(4) . . . . ? C5 N1 C1 C2 0.2(6) . . . . ? Cd1 N1 C1 C2 -164.6(4) . . . . ? N1 C1 C2 C3 1.7(7) . . . . ? C1 C2 C3 C4 -2.3(7) . . . . ? C2 C3 C4 C5 0.9(6) . . . . ? C2 C3 C4 C6 -177.6(4) . . . . ? C1 N1 C5 C4 -1.7(6) . . . . ? Cd1 N1 C5 C4 163.1(3) . . . . ? C3 C4 C5 N1 1.1(6) . . . . ? C6 C4 C5 N1 179.6(4) . . . . ? C3 C4 C6 O1 31.8(7) . . . . ? C5 C4 C6 O1 -146.7(5) . . . . ? C3 C4 C6 C7 -147.2(4) . . . . ? C5 C4 C6 C7 34.3(6) . . . . ? C11 N2 C7 C8 -2.3(6) . . . . ? C11 N2 C7 C6 174.1(3) . . . . ? O1 C6 C7 N2 -150.4(4) . . . . ? C4 C6 C7 N2 28.5(6) . . . . ? O1 C6 C7 C8 26.1(7) . . . . ? C4 C6 C7 C8 -154.9(4) . . . . ? N2 C7 C8 C9 -0.1(6) . . . . ? C6 C7 C8 C9 -176.4(4) . . . . ? C7 C8 C9 C10 2.3(7) . . . . ? C8 C9 C10 C11 -1.9(7) . . . . ? C7 N2 C11 C10 2.7(6) . . . . ? C7 N2 C11 C12 -175.0(3) . . . . ? C9 C10 C11 N2 -0.6(6) . . . . ? C9 C10 C11 C12 177.0(4) . . . . ? N2 C11 C12 O2 145.4(4) . . . . ? C10 C11 C12 O2 -32.3(6) . . . . ? N2 C11 C12 C13 -33.4(5) . . . . ? C10 C11 C12 C13 148.9(4) . . . . ? O2 C12 C13 C17 159.6(4) . . . . ? C11 C12 C13 C17 -21.6(6) . . . . ? O2 C12 C13 C14 -18.2(6) . . . . ? C11 C12 C13 C14 160.5(4) . . . . ? C17 C13 C14 C15 -0.1(6) . . . . ? C12 C13 C14 C15 177.9(4) . . . . ? C13 C14 C15 C16 1.6(6) . . . . ? C17 N3 C16 C15 -0.2(6) . . . . ? Cd1 N3 C16 C15 169.6(3) . . . . ? C14 C15 C16 N3 -1.5(7) . . . . ? C16 N3 C17 C13 1.9(6) . . . . ? Cd1 N3 C17 C13 -167.9(3) . . . . ? C14 C13 C17 N3 -1.8(6) . . . . ? C12 C13 C17 N3 -179.7(4) . . . . ? C22 N4 C18 C19 1.9(7) . . . . ? Cd2 N4 C18 C19 166.9(4) . . . . ? N4 C18 C19 C20 -1.9(8) . . . . ? C18 C19 C20 C21 -0.3(7) . . . . ? C19 C20 C21 C22 2.3(7) . . . . ? C19 C20 C21 C23 -176.9(5) . . . . ? C18 N4 C22 C21 0.2(6) . . . . ? Cd2 N4 C22 C21 -164.0(3) . . . . ? C20 C21 C22 N4 -2.4(7) . . . . ? C23 C21 C22 N4 176.8(4) . . . . ? C20 C21 C23 O3 -50.6(7) . . . . ? C22 C21 C23 O3 130.3(5) . . . . ? C20 C21 C23 C24 122.3(5) . . . . ? C22 C21 C23 C24 -56.9(6) . . . . ? C28 N5 C24 C25 1.2(8) . . . . ? C28 N5 C24 C23 -175.6(4) . . . . ? O3 C23 C24 N5 167.9(5) . . . . ? C21 C23 C24 N5 -5.0(7) . . . . ? O3 C23 C24 C25 -8.9(8) . . . . ? C21 C23 C24 C25 178.2(5) . . . . ? N5 C24 C25 C26 -2.4(9) . . . . ? C23 C24 C25 C26 174.3(6) . . . . ? C24 C25 C26 C27 1.5(11) . . . . ? C25 C26 C27 C28 0.5(12) . . . . ? C24 N5 C28 C27 0.9(8) . . . . ? C24 N5 C28 C29 179.1(5) . . . . ? C26 C27 C28 N5 -1.7(10) . . . . ? C26 C27 C28 C29 -180.0(7) . . . . ? N5 C28 C29 O4 -164.4(5) . . . . ? C27 C28 C29 O4 13.9(8) . . . . ? N5 C28 C29 C30 14.3(8) . . . . ? C27 C28 C29 C30 -167.4(5) . . . . ? O4 C29 C30 C34 -150.9(5) . . . . ? C28 C29 C30 C34 30.3(7) . . . . ? O4 C29 C30 C31 26.4(8) . . . . ? C28 C29 C30 C31 -152.3(5) . . . . ? C34 C30 C31 C32 0.9(8) . . . . ? C29 C30 C31 C32 -176.6(6) . . . . ? C30 C31 C32 C33 -1.1(10) . . . . ? C34 N6 C33 C32 1.1(9) . . . . ? Cd2 N6 C33 C32 -167.4(5) . . . . ? C31 C32 C33 N6 0.1(11) . . . . ? C33 N6 C34 C30 -1.4(7) . . . . ? Cd2 N6 C34 C30 166.7(3) . . . . ? C31 C30 C34 N6 0.4(7) . . . . ? C29 C30 C34 N6 177.8(4) . . . . ? O12 Cl2 O10 O11' 156.9(7) . . . . ? O9 Cl2 O10 O11' -94.5(6) . . . . ? O11 Cl2 O10 O11' 58.4(9) . . . . ? O12 Cl2 O11' O10 -65.8(15) . . . . ? O9 Cl2 O11' O10 109.5(5) . . . . ? O11 Cl2 O11' O10 -139.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.028 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.077 #####################################end####################### data_complex5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H18 Cd Cl2 N3 O13.50' _chemical_formula_weight 663.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.7355(10) _cell_length_b 10.0002(10) _cell_length_c 26.295(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2560.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.131 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.919851 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13968 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4504 _reflns_number_gt 3511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0923P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(6) _refine_ls_number_reflns 4504 _refine_ls_number_parameters 334 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1394 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.53138(7) 0.68658(6) 0.63384(2) 0.0358(2) Uani 1 1 d . . . N1 N 0.6494(8) 0.8471(7) 0.5879(2) 0.0369(18) Uani 1 1 d . . . C1 C 0.6941(9) 0.8153(10) 0.5402(3) 0.0375(19) Uani 1 1 d . . . H1A H 0.6742 0.7308 0.5274 0.045 Uiso 1 1 calc R . . C2 C 0.7672(10) 0.9025(9) 0.5103(3) 0.036(2) Uani 1 1 d . . . C3 C 0.7485(15) 1.0636(10) 0.5761(4) 0.064(3) Uani 1 1 d . . . H3A H 0.7615 1.1500 0.5882 0.077 Uiso 1 1 calc R . . C4 C 0.6768(12) 0.9708(10) 0.6044(3) 0.049(3) Uani 1 1 d . . . H4A H 0.6459 0.9954 0.6365 0.059 Uiso 1 1 calc R . . C5 C 0.8000(14) 1.0264(9) 0.5301(4) 0.058(3) Uani 1 1 d . . . H5A H 0.8571 1.0841 0.5122 0.070 Uiso 1 1 calc R . . C6 C 0.8241(11) 0.8610(9) 0.4599(3) 0.038(2) Uani 1 1 d . . . O2 O 0.9548(7) 0.6322(7) 0.3080(2) 0.0516(18) Uani 1 1 d . . . C7 C 0.7384(9) 0.7812(9) 0.4235(3) 0.035(2) Uani 1 1 d . . . C8 C 0.5964(10) 0.7728(10) 0.4268(4) 0.046(2) Uani 1 1 d . . . H8A H 0.5484 0.8159 0.4526 0.056 Uiso 1 1 calc R . . C9 C 0.5276(11) 0.6973(11) 0.3898(3) 0.053(2) Uani 1 1 d . . . H9A H 0.4321 0.6940 0.3893 0.063 Uiso 1 1 calc R . . C10 C 0.6029(10) 0.6280(10) 0.3541(3) 0.043(2) Uani 1 1 d . . . H10A H 0.5605 0.5712 0.3309 0.051 Uiso 1 1 calc R . . C11 C 0.7471(9) 0.6461(8) 0.3539(3) 0.034(2) Uani 1 1 d . . . N2 N 0.8113(7) 0.7237(7) 0.3869(2) 0.0320(17) Uani 1 1 d . . . C12 C 0.8395(10) 0.5823(10) 0.3152(3) 0.041(2) Uani 1 1 d . . . O1 O 0.9407(7) 0.8935(6) 0.4486(2) 0.0433(16) Uani 1 1 d . . . C13 C 0.7616(12) 0.2426(10) 0.2275(4) 0.053(3) Uani 1 1 d . . . H13A H 0.7473 0.1664 0.2079 0.064 Uiso 1 1 calc R . . C14 C 0.6994(12) 0.2512(10) 0.2739(4) 0.056(3) Uani 1 1 d . . . H14A H 0.6435 0.1816 0.2850 0.067 Uiso 1 1 calc R . . C15 C 0.7183(11) 0.3626(10) 0.3048(4) 0.049(3) Uani 1 1 d . . . H15A H 0.6783 0.3683 0.3369 0.058 Uiso 1 1 calc R . . C16 C 0.7996(9) 0.4651(9) 0.2856(3) 0.037(2) Uani 1 1 d . . . C17 C 0.8579(10) 0.4479(10) 0.2381(3) 0.042(2) Uani 1 1 d . . . H17A H 0.9120 0.5168 0.2253 0.050 Uiso 1 1 calc R . . N3 N 0.8416(8) 0.3386(8) 0.2093(3) 0.043(2) Uani 1 1 d . . . Cl1 Cl 0.6846(4) 0.8514(3) 0.23116(14) 0.0810(10) Uani 1 1 d D . . O3 O 0.8264(11) 0.8840(15) 0.2289(6) 0.149(5) Uani 1 1 d DU . . O4 O 0.6171(13) 0.9130(13) 0.1907(4) 0.122(4) Uani 1 1 d DU . . O5 O 0.6536(14) 0.7159(9) 0.2366(4) 0.115(4) Uani 1 1 d DU . . O6 O 0.639(2) 0.9023(17) 0.2789(5) 0.181(6) Uani 1 1 d DU . . Cl2 Cl 0.3352(4) 1.0646(4) 0.51943(14) 0.0817(10) Uani 1 1 d D . . O7 O 0.341(2) 1.0875(16) 0.5709(4) 0.164(6) Uani 1 1 d DU . . O8 O 0.424(2) 1.1591(18) 0.5000(8) 0.231(9) Uani 1 1 d DU . . O9 O 0.3828(13) 0.9387(9) 0.5088(4) 0.108(3) Uani 1 1 d DU . . O10 O 0.2144(18) 1.090(2) 0.4951(8) 0.255(10) Uani 1 1 d DU . . O1W O 0.3966(9) 0.5107(8) 0.6619(3) 0.072(2) Uani 1 1 d . . . O2W O 0.6902(10) 0.5320(9) 0.6036(3) 0.080(3) Uani 1 1 d . . . O3W O 0.4287(13) 1.0332(16) 0.3473(6) 0.163(6) Uani 1 1 d . . . O4W O 0.697(4) 1.123(2) 0.4097(8) 0.152(13) Uani 0.50 1 d P . . H1WB H 0.3444 0.4373 0.6605 0.228 Uiso 1 1 d R . . H2WB H 0.6355 0.4922 0.5827 0.228 Uiso 1 1 d R . . H2WA H 0.7584 0.4695 0.6090 0.228 Uiso 1 1 d R . . H1WA H 0.4186 0.5508 0.6940 0.228 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0337(3) 0.0486(4) 0.0252(3) 0.0035(3) -0.0013(3) 0.0053(3) N1 0.039(4) 0.046(5) 0.025(4) 0.003(3) 0.001(3) -0.002(3) C1 0.038(5) 0.047(5) 0.028(4) -0.004(4) 0.002(3) 0.005(5) C2 0.036(5) 0.042(5) 0.029(4) -0.005(4) 0.011(4) 0.000(4) C3 0.122(11) 0.033(5) 0.036(6) -0.011(5) 0.002(6) -0.004(6) C4 0.068(7) 0.050(6) 0.028(5) -0.016(4) 0.003(5) 0.010(5) C5 0.104(10) 0.033(5) 0.036(5) 0.000(4) 0.015(6) -0.014(6) C6 0.047(6) 0.038(5) 0.029(5) 0.012(4) 0.005(4) 0.003(4) O2 0.039(4) 0.074(4) 0.042(4) -0.025(3) 0.014(3) -0.021(4) C7 0.035(5) 0.050(6) 0.020(4) 0.001(3) 0.002(4) 0.000(4) C8 0.036(5) 0.063(6) 0.041(5) -0.009(4) 0.004(4) -0.001(5) C9 0.029(4) 0.083(7) 0.045(5) -0.019(5) 0.001(4) 0.000(6) C10 0.031(5) 0.055(5) 0.042(6) -0.008(4) 0.005(4) -0.006(4) C11 0.038(5) 0.037(5) 0.027(5) -0.004(3) 0.000(3) -0.004(4) N2 0.032(4) 0.046(4) 0.018(3) -0.002(3) 0.001(3) -0.002(3) C12 0.036(6) 0.051(6) 0.037(5) -0.006(4) -0.002(4) -0.007(5) O1 0.043(5) 0.055(4) 0.032(3) -0.007(3) 0.012(3) -0.009(3) C13 0.056(7) 0.045(6) 0.060(7) -0.012(5) 0.017(6) -0.009(5) C14 0.068(8) 0.041(6) 0.059(7) 0.003(5) 0.013(6) -0.017(5) C15 0.049(6) 0.052(6) 0.044(6) 0.002(5) 0.019(5) 0.003(5) C16 0.038(5) 0.037(5) 0.035(5) -0.010(4) 0.004(4) 0.002(4) C17 0.042(6) 0.048(6) 0.035(5) -0.006(4) 0.004(4) -0.004(5) N3 0.039(4) 0.056(5) 0.034(4) -0.018(4) 0.009(3) 0.000(4) Cl1 0.086(3) 0.069(2) 0.088(2) 0.0214(18) -0.019(2) -0.0044(17) O3 0.110(8) 0.169(9) 0.167(9) 0.030(8) -0.018(7) -0.013(7) O4 0.112(7) 0.131(8) 0.122(7) 0.055(6) -0.031(6) 0.006(6) O5 0.138(8) 0.083(6) 0.122(7) 0.000(5) -0.020(6) 0.002(6) O6 0.213(11) 0.176(9) 0.156(9) -0.038(8) 0.025(8) 0.010(8) Cl2 0.095(3) 0.070(2) 0.080(2) 0.0080(18) -0.0103(19) 0.003(2) O7 0.202(10) 0.154(9) 0.137(8) -0.044(7) -0.008(8) 0.002(8) O8 0.236(12) 0.202(11) 0.254(12) 0.008(9) 0.033(9) -0.031(9) O9 0.131(8) 0.075(6) 0.117(6) -0.003(5) 0.020(6) 0.007(6) O10 0.225(13) 0.277(13) 0.263(13) -0.030(10) -0.038(10) 0.037(10) O1W 0.063(5) 0.071(5) 0.081(5) 0.015(4) -0.011(5) -0.019(4) O2W 0.083(6) 0.105(7) 0.052(5) -0.008(4) -0.003(4) 0.054(6) O3W 0.090(10) 0.211(15) 0.189(13) 0.092(11) -0.014(8) -0.056(10) O4W 0.29(4) 0.083(14) 0.088(15) 0.013(11) -0.07(2) 0.047(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N1 2.314(7) . ? Cd1 O1W 2.315(8) . ? Cd1 O2W 2.326(8) . ? Cd1 N3 2.351(7) 2_665 ? Cd1 N2 2.386(7) 4_466 ? Cd1 O1 2.473(6) 4_466 ? Cd1 O2 2.485(6) 4_466 ? N1 C4 1.338(12) . ? N1 C1 1.363(10) . ? C1 C2 1.373(13) . ? C1 H1A 0.9300 . ? C2 C5 1.382(13) . ? C2 C6 1.495(12) . ? C3 C5 1.360(14) . ? C3 C4 1.380(15) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 O1 1.218(11) . ? C6 C7 1.499(12) . ? O2 C12 1.242(11) . ? O2 Cd1 2.485(6) 4_566 ? C7 N2 1.327(10) . ? C7 C8 1.388(13) . ? C8 C9 1.402(13) . ? C8 H8A 0.9300 . ? C9 C10 1.378(13) . ? C9 H9A 0.9300 . ? C10 C11 1.416(13) . ? C10 H10A 0.9300 . ? C11 N2 1.321(10) . ? C11 C12 1.502(12) . ? N2 Cd1 2.386(7) 4_566 ? C12 C16 1.459(12) . ? O1 Cd1 2.473(5) 4_566 ? C13 N3 1.326(13) . ? C13 C14 1.366(15) . ? C13 H13A 0.9300 . ? C14 C15 1.392(14) . ? C14 H14A 0.9300 . ? C15 C16 1.390(13) . ? C15 H15A 0.9300 . ? C16 C17 1.384(12) . ? C17 N3 1.339(11) . ? C17 H17A 0.9300 . ? N3 Cd1 2.351(7) 2_664 ? Cl1 O4 1.394(8) . ? Cl1 O5 1.396(9) . ? Cl1 O3 1.420(10) . ? Cl1 O6 1.426(10) . ? Cl2 O10 1.363(12) . ? Cl2 O9 1.370(9) . ? Cl2 O7 1.373(10) . ? Cl2 O8 1.379(12) . ? O1W H1WB 0.8939 . ? O1W H1WA 0.9573 . ? O2W H2WB 0.8638 . ? O2W H2WA 0.9229 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 O1W 167.1(3) . . ? N1 Cd1 O2W 87.3(3) . . ? O1W Cd1 O2W 88.9(4) . . ? N1 Cd1 N3 104.7(3) . 2_665 ? O1W Cd1 N3 87.0(3) . 2_665 ? O2W Cd1 N3 82.4(3) . 2_665 ? N1 Cd1 N2 93.7(3) . 4_466 ? O1W Cd1 N2 81.4(3) . 4_466 ? O2W Cd1 N2 140.2(3) . 4_466 ? N3 Cd1 N2 134.9(2) 2_665 4_466 ? N1 Cd1 O1 86.8(2) . 4_466 ? O1W Cd1 O1 80.3(3) . 4_466 ? O2W Cd1 O1 73.9(3) . 4_466 ? N3 Cd1 O1 153.2(3) 2_665 4_466 ? N2 Cd1 O1 66.5(2) 4_466 4_466 ? N1 Cd1 O2 88.0(3) . 4_466 ? O1W Cd1 O2 100.8(3) . 4_466 ? O2W Cd1 O2 153.4(3) . 4_466 ? N3 Cd1 O2 73.5(2) 2_665 4_466 ? N2 Cd1 O2 66.2(2) 4_466 4_466 ? O1 Cd1 O2 131.9(2) 4_466 4_466 ? C4 N1 C1 116.7(8) . . ? C4 N1 Cd1 124.8(6) . . ? C1 N1 Cd1 118.5(6) . . ? N1 C1 C2 123.0(9) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C1 C2 C5 118.2(8) . . ? C1 C2 C6 121.6(8) . . ? C5 C2 C6 119.9(8) . . ? C5 C3 C4 118.8(9) . . ? C5 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? N1 C4 C3 123.2(9) . . ? N1 C4 H4A 118.4 . . ? C3 C4 H4A 118.4 . . ? C3 C5 C2 119.7(10) . . ? C3 C5 H5A 120.2 . . ? C2 C5 H5A 120.2 . . ? O1 C6 C2 119.2(8) . . ? O1 C6 C7 120.3(8) . . ? C2 C6 C7 120.5(8) . . ? C12 O2 Cd1 118.1(6) . 4_566 ? N2 C7 C8 123.4(8) . . ? N2 C7 C6 113.3(8) . . ? C8 C7 C6 123.2(8) . . ? C7 C8 C9 117.8(9) . . ? C7 C8 H8A 121.1 . . ? C9 C8 H8A 121.1 . . ? C10 C9 C8 119.3(10) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? C9 C10 C11 117.7(9) . . ? C9 C10 H10A 121.1 . . ? C11 C10 H10A 121.1 . . ? N2 C11 C10 122.9(8) . . ? N2 C11 C12 114.3(8) . . ? C10 C11 C12 122.8(8) . . ? C11 N2 C7 118.5(8) . . ? C11 N2 Cd1 119.7(5) . 4_566 ? C7 N2 Cd1 118.9(6) . 4_566 ? O2 C12 C16 118.9(8) . . ? O2 C12 C11 118.2(8) . . ? C16 C12 C11 122.9(8) . . ? C6 O1 Cd1 117.4(6) . 4_566 ? N3 C13 C14 122.5(9) . . ? N3 C13 H13A 118.7 . . ? C14 C13 H13A 118.7 . . ? C13 C14 C15 120.9(9) . . ? C13 C14 H14A 119.5 . . ? C15 C14 H14A 119.5 . . ? C16 C15 C14 117.0(9) . . ? C16 C15 H15A 121.5 . . ? C14 C15 H15A 121.5 . . ? C17 C16 C15 118.1(8) . . ? C17 C16 C12 118.1(9) . . ? C15 C16 C12 123.4(8) . . ? N3 C17 C16 124.3(9) . . ? N3 C17 H17A 117.8 . . ? C16 C17 H17A 117.8 . . ? C13 N3 C17 117.2(8) . . ? C13 N3 Cd1 122.4(6) . 2_664 ? C17 N3 Cd1 120.2(6) . 2_664 ? O4 Cl1 O5 113.9(8) . . ? O4 Cl1 O3 109.0(8) . . ? O5 Cl1 O3 115.9(9) . . ? O4 Cl1 O6 111.5(10) . . ? O5 Cl1 O6 100.9(9) . . ? O3 Cl1 O6 105.0(11) . . ? O10 Cl2 O9 111.5(12) . . ? O10 Cl2 O7 117.7(14) . . ? O9 Cl2 O7 110.0(9) . . ? O10 Cl2 O8 103.8(14) . . ? O9 Cl2 O8 110.0(11) . . ? O7 Cl2 O8 103.1(12) . . ? Cd1 O1W H1WB 158.9 . . ? Cd1 O1W H1WA 80.6 . . ? H1WB O1W H1WA 120.5 . . ? Cd1 O2W H2WB 96.6 . . ? Cd1 O2W H2WA 151.2 . . ? H2WB O2W H2WA 103.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1W Cd1 N1 C4 147.9(13) . . . . ? O2W Cd1 N1 C4 -139.1(8) . . . . ? N3 Cd1 N1 C4 -57.7(8) 2_665 . . . ? N2 Cd1 N1 C4 80.7(8) 4_466 . . . ? O1 Cd1 N1 C4 146.9(8) 4_466 . . . ? O2 Cd1 N1 C4 14.7(8) 4_466 . . . ? O1W Cd1 N1 C1 -31.5(17) . . . . ? O2W Cd1 N1 C1 41.5(6) . . . . ? N3 Cd1 N1 C1 122.9(6) 2_665 . . . ? N2 Cd1 N1 C1 -98.7(6) 4_466 . . . ? O1 Cd1 N1 C1 -32.6(6) 4_466 . . . ? O2 Cd1 N1 C1 -164.7(6) 4_466 . . . ? C4 N1 C1 C2 1.8(13) . . . . ? Cd1 N1 C1 C2 -178.7(7) . . . . ? N1 C1 C2 C5 1.9(15) . . . . ? N1 C1 C2 C6 175.2(8) . . . . ? C1 N1 C4 C3 -1.1(15) . . . . ? Cd1 N1 C4 C3 179.4(9) . . . . ? C5 C3 C4 N1 -3.3(19) . . . . ? C4 C3 C5 C2 7.1(19) . . . . ? C1 C2 C5 C3 -6.4(17) . . . . ? C6 C2 C5 C3 -179.7(11) . . . . ? C1 C2 C6 O1 -136.2(9) . . . . ? C5 C2 C6 O1 36.9(14) . . . . ? C1 C2 C6 C7 44.2(13) . . . . ? C5 C2 C6 C7 -142.7(10) . . . . ? O1 C6 C7 N2 16.5(12) . . . . ? C2 C6 C7 N2 -164.0(8) . . . . ? O1 C6 C7 C8 -161.1(9) . . . . ? C2 C6 C7 C8 18.4(13) . . . . ? N2 C7 C8 C9 1.2(15) . . . . ? C6 C7 C8 C9 178.6(8) . . . . ? C7 C8 C9 C10 4.2(15) . . . . ? C8 C9 C10 C11 -5.4(15) . . . . ? C9 C10 C11 N2 1.4(14) . . . . ? C9 C10 C11 C12 -176.5(9) . . . . ? C10 C11 N2 C7 3.9(13) . . . . ? C12 C11 N2 C7 -178.1(8) . . . . ? C10 C11 N2 Cd1 -156.8(7) . . . 4_566 ? C12 C11 N2 Cd1 21.3(10) . . . 4_566 ? C8 C7 N2 C11 -5.2(13) . . . . ? C6 C7 N2 C11 177.1(7) . . . . ? C8 C7 N2 Cd1 155.5(7) . . . 4_566 ? C6 C7 N2 Cd1 -22.1(9) . . . 4_566 ? Cd1 O2 C12 C16 -172.5(6) 4_566 . . . ? Cd1 O2 C12 C11 7.7(11) 4_566 . . . ? N2 C11 C12 O2 -19.1(12) . . . . ? C10 C11 C12 O2 159.0(9) . . . . ? N2 C11 C12 C16 161.1(8) . . . . ? C10 C11 C12 C16 -20.8(14) . . . . ? C2 C6 O1 Cd1 177.5(6) . . . 4_566 ? C7 C6 O1 Cd1 -2.9(10) . . . 4_566 ? N3 C13 C14 C15 -0.4(19) . . . . ? C13 C14 C15 C16 1.8(17) . . . . ? C14 C15 C16 C17 -1.4(15) . . . . ? C14 C15 C16 C12 -174.0(10) . . . . ? O2 C12 C16 C17 -27.5(14) . . . . ? C11 C12 C16 C17 152.4(9) . . . . ? O2 C12 C16 C15 145.1(10) . . . . ? C11 C12 C16 C15 -35.1(14) . . . . ? C15 C16 C17 N3 -0.2(15) . . . . ? C12 C16 C17 N3 172.8(9) . . . . ? C14 C13 N3 C17 -1.2(17) . . . . ? C14 C13 N3 Cd1 172.8(9) . . . 2_664 ? C16 C17 N3 C13 1.6(15) . . . . ? C16 C17 N3 Cd1 -172.6(7) . . . 2_664 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.981 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.124 #################################end######################## data_complex6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H29.6 Cd N6 O11.80 S' _chemical_formula_weight 855.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.674(3) _cell_length_b 9.1071(16) _cell_length_c 24.873(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.219(4) _cell_angle_gamma 90.00 _cell_volume 3587.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1714 _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type multi-Scan _exptl_absorpt_correction_T_min 0.467919 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ASDABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18867 _diffrn_reflns_av_R_equivalents 0.0946 _diffrn_reflns_av_sigmaI/netI 0.1124 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6320 _reflns_number_gt 3642 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELTXL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+0.7550P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6320 _refine_ls_number_parameters 485 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.1281 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1872 _refine_ls_wR_factor_gt 0.1526 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.49952(3) 0.33919(6) 0.32116(2) 0.0341(2) Uani 1 1 d . . . N1 N 0.3609(4) 0.2384(7) 0.2785(3) 0.0368(16) Uani 1 1 d . . . N2 N 0.2120(4) 0.5029(7) 0.3387(3) 0.0348(15) Uani 1 1 d . . . N3 N 0.4581(4) 0.3785(7) 0.4030(3) 0.0372(16) Uani 1 1 d . . . N4 N 0.6267(4) 0.4721(8) 0.3656(3) 0.0363(16) Uani 1 1 d . . . N5 N 0.8680(4) 0.5849(8) 0.5387(3) 0.0442(17) Uani 1 1 d . . . O1 O 0.0732(4) 0.3683(7) 0.2118(3) 0.068(2) Uani 1 1 d . . . O2 O 0.2800(4) 0.6655(7) 0.4727(3) 0.0586(17) Uani 1 1 d . . . O3 O 0.8567(4) 0.2741(9) 0.4530(3) 0.079(2) Uani 1 1 d . . . O4 O 0.9107(4) 0.8021(8) 0.6622(3) 0.071(2) Uani 1 1 d . . . C1 C 0.2951(5) 0.3310(9) 0.2716(3) 0.0370(19) Uani 1 1 d . . . H1A H 0.3060 0.4306 0.2784 0.044 Uiso 1 1 calc R . . C2 C 0.2114(4) 0.2830(9) 0.2549(3) 0.0347(18) Uani 1 1 d . . . C3 C 0.1964(6) 0.1341(9) 0.2438(3) 0.048(2) Uani 1 1 d . . . H3A H 0.1413 0.0987 0.2325 0.058 Uiso 1 1 calc R . . C4 C 0.2627(6) 0.0391(10) 0.2497(4) 0.053(2) Uani 1 1 d . . . H4A H 0.2532 -0.0604 0.2418 0.064 Uiso 1 1 calc R . . C5 C 0.3441(6) 0.0954(10) 0.2679(3) 0.046(2) Uani 1 1 d . . . H5A H 0.3891 0.0310 0.2729 0.055 Uiso 1 1 calc R . . C6 C 0.1411(5) 0.3874(10) 0.2493(4) 0.045(2) Uani 1 1 d . . . C7 C 0.1524(4) 0.5163(9) 0.2881(4) 0.042(2) Uani 1 1 d . . . C8 C 0.1016(5) 0.6379(10) 0.2732(4) 0.056(3) Uani 1 1 d . . . H8A H 0.0600 0.6426 0.2381 0.068 Uiso 1 1 calc R . . C9 C 0.1128(6) 0.7535(11) 0.3110(5) 0.068(3) Uani 1 1 d . . . H9A H 0.0805 0.8385 0.3017 0.082 Uiso 1 1 calc R . . C10 C 0.1728(5) 0.7384(10) 0.3624(4) 0.054(2) Uani 1 1 d . . . H10A H 0.1811 0.8136 0.3889 0.065 Uiso 1 1 calc R . . C11 C 0.2213(5) 0.6136(9) 0.3758(4) 0.039(2) Uani 1 1 d . . . C12 C 0.2848(5) 0.5938(9) 0.4328(4) 0.039(2) Uani 1 1 d . . . C13 C 0.4872(5) 0.3026(9) 0.4514(3) 0.047(2) Uani 1 1 d . . . H13A H 0.5320 0.2383 0.4554 0.056 Uiso 1 1 calc R . . C14 C 0.4540(6) 0.3147(9) 0.4959(4) 0.052(2) Uani 1 1 d . . . H14A H 0.4770 0.2618 0.5291 0.063 Uiso 1 1 calc R . . C15 C 0.3867(5) 0.4061(9) 0.4898(3) 0.044(2) Uani 1 1 d . . . H15A H 0.3624 0.4143 0.5186 0.052 Uiso 1 1 calc R . . C16 C 0.3545(4) 0.4871(8) 0.4401(3) 0.0330(18) Uani 1 1 d . . . C17 C 0.3935(4) 0.4697(8) 0.3982(3) 0.0332(18) Uani 1 1 d . . . H17A H 0.3733 0.5246 0.3652 0.040 Uiso 1 1 calc R . . N6 N 0.6732(3) 0.9629(6) 0.5674(3) 0.071(2) Uani 1 1 d G . . C34 C 0.6668(4) 1.0094(7) 0.5130(3) 0.097(3) Uani 1 1 d GU . . H34A H 0.6199 1.0629 0.4920 0.117 Uiso 1 1 calc RU . . C33 C 0.7305(5) 0.9760(8) 0.4898(2) 0.093(3) Uani 1 1 d GU . . H33A H 0.7262 1.0071 0.4534 0.111 Uiso 1 1 calc RU . . C32 C 0.8005(4) 0.8960(7) 0.5211(3) 0.066(3) Uani 1 1 d G . . H32A H 0.8431 0.8736 0.5057 0.080 Uiso 1 1 calc R . . C31 C 0.8069(3) 0.8494(6) 0.5755(2) 0.050(2) Uani 1 1 d G . . C30 C 0.7432(4) 0.8829(6) 0.5987(2) 0.057(3) Uani 1 1 d G . . H30A H 0.7475 0.8518 0.6351 0.069 Uiso 1 1 calc R . . C29 C 0.8805(5) 0.7662(11) 0.6132(4) 0.054(2) Uani 1 1 d . . . C28 C 0.9135(5) 0.6369(10) 0.5891(4) 0.047(2) Uani 1 1 d . . . C27 C 0.9865(6) 0.5708(14) 0.6222(4) 0.068(3) Uani 1 1 d . . . H27A H 1.0168 0.6108 0.6570 0.082 Uiso 1 1 calc R . . C26 C 1.0140(6) 0.4449(14) 0.6030(4) 0.075(3) Uani 1 1 d . . . H26A H 1.0627 0.3975 0.6247 0.090 Uiso 1 1 calc R . . C25 C 0.9677(5) 0.3903(12) 0.5507(4) 0.064(3) Uani 1 1 d . . . H25A H 0.9849 0.3060 0.5363 0.077 Uiso 1 1 calc R . . C24 C 0.8948(5) 0.4643(11) 0.5202(3) 0.047(2) Uani 1 1 d . . . C23 C 0.8419(5) 0.3970(11) 0.4659(4) 0.049(2) Uani 1 1 d . . . C22 C 0.6955(5) 0.4073(10) 0.3999(3) 0.041(2) Uani 1 1 d . . . H22A H 0.6936 0.3069 0.4062 0.050 Uiso 1 1 calc R . . C21 C 0.7694(5) 0.4819(10) 0.4266(3) 0.043(2) Uani 1 1 d . . . C20 C 0.7725(5) 0.6293(11) 0.4162(4) 0.054(3) Uani 1 1 d . . . H20A H 0.8209 0.6831 0.4341 0.065 Uiso 1 1 calc R . . C19 C 0.7035(5) 0.6975(10) 0.3788(3) 0.051(2) Uani 1 1 d . . . H19A H 0.7055 0.7962 0.3698 0.061 Uiso 1 1 calc R . . C18 C 0.6313(5) 0.6158(10) 0.3553(3) 0.043(2) Uani 1 1 d . . . H18A H 0.5840 0.6623 0.3313 0.052 Uiso 1 1 calc R . . S1 S 0.60053(12) 0.1783(2) 0.23997(9) 0.0440(6) Uani 1 1 d DU . . O5 O 0.6569(5) 0.1378(11) 0.2951(3) 0.123(3) Uani 1 1 d DU . . O6 O 0.6490(5) 0.2226(9) 0.2053(4) 0.106(3) Uani 1 1 d DU . . O7 O 0.5518(4) 0.0516(6) 0.2178(3) 0.0735(19) Uani 1 1 d DU . . O8 O 0.5439(4) 0.2947(6) 0.2466(2) 0.0509(15) Uani 1 1 d DU . . O1W O 0.9121(9) -0.0977(16) 0.4146(7) 0.105(5) Uani 0.60 1 d P . . O1W' O 0.9812(15) -0.015(3) 0.4278(18) 0.23(2) Uani 0.40 1 d P . . O3W O 0.4505(5) -0.0865(8) 0.3883(3) 0.083(2) Uani 1 1 d . . . O4W O 0.5553(4) 0.1142(7) 0.3628(3) 0.068(2) Uani 1 1 d . . . O2W O 0.8167(8) 0.118(2) 0.3494(6) 0.250(12) Uani 0.80 1 d P . . H4WA H 0.5871 0.1225 0.3408 0.375 Uiso 1 1 d R . . H4WB H 0.5422 0.0271 0.3763 0.375 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0319(3) 0.0333(4) 0.0372(4) 0.0000(3) 0.0112(3) 0.0050(3) N1 0.044(4) 0.033(4) 0.037(4) -0.001(3) 0.019(3) 0.006(3) N2 0.028(3) 0.040(4) 0.038(4) 0.007(3) 0.012(3) 0.004(3) N3 0.034(3) 0.043(4) 0.031(4) 0.002(3) 0.004(3) 0.006(3) N4 0.032(4) 0.044(5) 0.032(4) -0.003(3) 0.008(3) 0.000(3) N5 0.033(4) 0.056(5) 0.039(4) -0.005(4) 0.005(3) -0.004(3) O1 0.039(3) 0.084(5) 0.060(4) -0.003(4) -0.014(3) -0.007(3) O2 0.075(4) 0.050(4) 0.057(4) -0.021(3) 0.031(4) 0.004(3) O3 0.061(4) 0.077(5) 0.083(5) -0.024(4) -0.002(4) 0.024(4) O4 0.064(4) 0.099(6) 0.040(4) -0.022(4) 0.001(3) -0.015(4) C1 0.042(4) 0.039(5) 0.030(4) -0.002(4) 0.010(4) -0.003(4) C2 0.033(4) 0.037(5) 0.030(4) 0.004(4) 0.005(4) -0.003(4) C3 0.051(5) 0.048(6) 0.042(5) -0.005(4) 0.009(4) -0.016(4) C4 0.070(6) 0.038(5) 0.048(6) -0.010(4) 0.011(5) -0.013(5) C5 0.064(6) 0.035(5) 0.038(5) -0.004(4) 0.012(5) 0.002(4) C6 0.039(5) 0.048(6) 0.046(5) 0.008(4) 0.009(4) -0.002(4) C7 0.025(4) 0.047(6) 0.049(5) 0.006(4) 0.002(4) 0.004(4) C8 0.036(5) 0.063(7) 0.062(6) 0.013(5) 0.005(5) 0.015(5) C9 0.053(6) 0.046(7) 0.100(9) 0.014(6) 0.018(6) 0.023(5) C10 0.039(5) 0.051(6) 0.076(7) -0.005(5) 0.024(5) 0.012(4) C11 0.034(4) 0.038(5) 0.049(6) 0.002(4) 0.018(4) 0.005(4) C12 0.040(5) 0.036(5) 0.046(5) -0.008(4) 0.019(4) -0.005(4) C13 0.047(5) 0.053(6) 0.039(5) 0.012(4) 0.011(4) 0.014(4) C14 0.069(6) 0.039(6) 0.036(5) 0.005(4) -0.001(5) -0.002(5) C15 0.058(5) 0.045(5) 0.031(5) -0.005(4) 0.017(4) -0.007(5) C16 0.037(4) 0.035(5) 0.027(4) -0.002(4) 0.010(4) -0.003(4) C17 0.032(4) 0.035(5) 0.028(4) 0.000(4) 0.003(4) -0.003(4) N6 0.081(6) 0.044(5) 0.084(6) -0.012(5) 0.020(5) 0.002(4) C34 0.119(7) 0.071(6) 0.090(6) 0.000(5) 0.015(6) 0.012(6) C33 0.125(6) 0.066(6) 0.075(6) 0.005(5) 0.015(5) 0.009(6) C32 0.103(8) 0.048(6) 0.052(6) -0.002(5) 0.031(6) 0.002(6) C31 0.069(6) 0.034(5) 0.046(6) -0.002(4) 0.015(5) -0.006(5) C30 0.063(6) 0.046(6) 0.059(6) -0.008(5) 0.015(5) -0.001(5) C29 0.047(5) 0.062(7) 0.051(6) 0.004(5) 0.013(5) -0.018(5) C28 0.032(4) 0.068(7) 0.043(5) 0.002(5) 0.014(4) -0.005(4) C27 0.046(6) 0.104(9) 0.045(6) -0.004(6) 0.000(5) -0.003(6) C26 0.040(5) 0.129(11) 0.044(6) 0.001(6) -0.004(5) 0.031(6) C25 0.048(5) 0.097(8) 0.043(6) 0.004(5) 0.007(5) 0.024(5) C24 0.034(5) 0.062(6) 0.039(5) 0.001(5) 0.005(4) -0.003(4) C23 0.034(5) 0.060(6) 0.050(6) -0.005(5) 0.009(4) 0.003(4) C22 0.040(5) 0.043(5) 0.041(5) 0.000(4) 0.013(4) 0.006(4) C21 0.038(5) 0.048(6) 0.047(5) -0.003(4) 0.016(4) 0.002(4) C20 0.042(5) 0.077(8) 0.044(6) -0.015(5) 0.013(5) -0.007(5) C19 0.059(6) 0.050(6) 0.040(5) 0.005(4) 0.012(5) 0.002(5) C18 0.040(5) 0.053(6) 0.029(5) -0.009(4) 0.000(4) 0.003(4) S1 0.0383(11) 0.0424(13) 0.0549(14) -0.0211(11) 0.0199(11) -0.0089(10) O5 0.075(5) 0.197(9) 0.073(5) -0.037(6) -0.010(4) 0.063(5) O6 0.133(6) 0.066(5) 0.171(8) -0.015(5) 0.122(6) -0.013(5) O7 0.051(3) 0.038(4) 0.126(5) -0.028(4) 0.021(4) -0.014(3) O8 0.067(4) 0.043(3) 0.055(4) -0.011(3) 0.036(3) 0.006(3) O1W 0.105(11) 0.071(10) 0.145(13) 0.013(9) 0.049(10) 0.006(8) O1W' 0.085(17) 0.065(18) 0.53(6) -0.01(3) 0.08(3) 0.012(14) O3W 0.106(6) 0.075(5) 0.075(5) 0.029(4) 0.037(4) 0.018(4) O4W 0.076(4) 0.054(4) 0.083(5) 0.028(4) 0.035(4) 0.038(3) O2W 0.142(11) 0.39(3) 0.136(11) -0.181(14) -0.069(9) 0.164(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O7 2.213(6) 2_655 ? Cd1 O8 2.238(5) . ? Cd1 O4W 2.352(6) . ? Cd1 N3 2.373(6) . ? Cd1 N4 2.391(6) . ? Cd1 N1 2.404(6) . ? N1 C5 1.341(10) . ? N1 C1 1.351(9) . ? N2 C11 1.342(10) . ? N2 C7 1.344(9) . ? N3 C17 1.335(9) . ? N3 C13 1.341(9) . ? N4 C22 1.335(9) . ? N4 C18 1.340(10) . ? N5 C24 1.321(11) . ? N5 C28 1.334(10) . ? O1 C6 1.234(9) . ? O2 C12 1.212(9) . ? O3 C23 1.210(11) . ? O4 C29 1.209(10) . ? C1 C2 1.396(10) . ? C1 H1A 0.9300 . ? C2 C3 1.390(11) . ? C2 C6 1.482(11) . ? C3 C4 1.376(12) . ? C3 H3A 0.9300 . ? C4 C5 1.388(11) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 C7 1.492(12) . ? C7 C8 1.373(11) . ? C8 C9 1.386(13) . ? C8 H8A 0.9300 . ? C9 C10 1.361(13) . ? C9 H9A 0.9300 . ? C10 C11 1.374(11) . ? C10 H10A 0.9300 . ? C11 C12 1.492(11) . ? C12 C16 1.482(10) . ? C13 C14 1.386(12) . ? C13 H13A 0.9300 . ? C14 C15 1.367(12) . ? C14 H14A 0.9300 . ? C15 C16 1.393(10) . ? C15 H15A 0.9300 . ? C16 C17 1.399(9) . ? C17 H17A 0.9300 . ? N6 C34 1.3900 . ? N6 C30 1.3900 . ? C34 C33 1.3900 . ? C34 H34A 0.9300 . ? C33 C32 1.3900 . ? C33 H33A 0.9300 . ? C32 C31 1.3900 . ? C32 H32A 0.9300 . ? C31 C30 1.3900 . ? C31 C29 1.497(11) . ? C30 H30A 0.9300 . ? C29 C28 1.502(13) . ? C28 C27 1.376(12) . ? C27 C26 1.375(15) . ? C27 H27A 0.9300 . ? C26 C25 1.380(13) . ? C26 H26A 0.9300 . ? C25 C24 1.390(11) . ? C25 H25A 0.9300 . ? C24 C23 1.495(11) . ? C23 C21 1.508(11) . ? C22 C21 1.382(11) . ? C22 H22A 0.9300 . ? C21 C20 1.371(12) . ? C20 C19 1.380(12) . ? C20 H20A 0.9300 . ? C19 C18 1.379(11) . ? C19 H19A 0.9300 . ? C18 H18A 0.9300 . ? S1 O6 1.414(7) . ? S1 O7 1.419(6) . ? S1 O5 1.447(7) . ? S1 O8 1.463(5) . ? O7 Cd1 2.213(5) 2_645 ? O1W O1W' 1.33(3) . ? O4W H4WA 0.8768 . ? O4W H4WB 0.9143 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Cd1 O8 88.8(2) 2_655 . ? O7 Cd1 O4W 179.5(2) 2_655 . ? O8 Cd1 O4W 91.1(2) . . ? O7 Cd1 N3 93.8(2) 2_655 . ? O8 Cd1 N3 177.1(2) . . ? O4W Cd1 N3 86.3(2) . . ? O7 Cd1 N4 85.7(2) 2_655 . ? O8 Cd1 N4 90.0(2) . . ? O4W Cd1 N4 93.8(2) . . ? N3 Cd1 N4 88.9(2) . . ? O7 Cd1 N1 87.3(2) 2_655 . ? O8 Cd1 N1 94.9(2) . . ? O4W Cd1 N1 93.2(2) . . ? N3 Cd1 N1 86.5(2) . . ? N4 Cd1 N1 171.4(2) . . ? C5 N1 C1 118.0(7) . . ? C5 N1 Cd1 124.8(5) . . ? C1 N1 Cd1 116.6(5) . . ? C11 N2 C7 117.9(7) . . ? C17 N3 C13 117.1(7) . . ? C17 N3 Cd1 117.4(5) . . ? C13 N3 Cd1 124.9(5) . . ? C22 N4 C18 117.6(7) . . ? C22 N4 Cd1 122.2(6) . . ? C18 N4 Cd1 120.1(5) . . ? C24 N5 C28 117.9(7) . . ? N1 C1 C2 122.6(7) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 117.8(7) . . ? C3 C2 C6 121.2(7) . . ? C1 C2 C6 121.0(7) . . ? C4 C3 C2 120.2(8) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 118.3(8) . . ? C3 C4 H4A 120.8 . . ? C5 C4 H4A 120.8 . . ? N1 C5 C4 123.1(8) . . ? N1 C5 H5A 118.5 . . ? C4 C5 H5A 118.5 . . ? O1 C6 C2 119.4(8) . . ? O1 C6 C7 120.0(8) . . ? C2 C6 C7 120.6(7) . . ? N2 C7 C8 122.6(8) . . ? N2 C7 C6 116.1(7) . . ? C8 C7 C6 121.2(8) . . ? C7 C8 C9 119.2(9) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? C10 C9 C8 117.7(9) . . ? C10 C9 H9A 121.2 . . ? C8 C9 H9A 121.2 . . ? C9 C10 C11 121.0(9) . . ? C9 C10 H10A 119.5 . . ? C11 C10 H10A 119.5 . . ? N2 C11 C10 121.5(8) . . ? N2 C11 C12 117.3(7) . . ? C10 C11 C12 121.2(8) . . ? O2 C12 C16 120.2(8) . . ? O2 C12 C11 120.4(7) . . ? C16 C12 C11 119.5(7) . . ? N3 C13 C14 123.5(8) . . ? N3 C13 H13A 118.3 . . ? C14 C13 H13A 118.3 . . ? C15 C14 C13 118.6(8) . . ? C15 C14 H14A 120.7 . . ? C13 C14 H14A 120.7 . . ? C14 C15 C16 119.7(8) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C15 C16 C17 117.4(7) . . ? C15 C16 C12 121.7(7) . . ? C17 C16 C12 120.8(7) . . ? N3 C17 C16 123.6(7) . . ? N3 C17 H17A 118.2 . . ? C16 C17 H17A 118.2 . . ? C34 N6 C30 120.0 . . ? N6 C34 C33 120.0 . . ? N6 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C31 C32 C33 120.0 . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 C29 124.2(5) . . ? C30 C31 C29 115.7(5) . . ? C31 C30 N6 120.0 . . ? C31 C30 H30A 120.0 . . ? N6 C30 H30A 120.0 . . ? O4 C29 C31 119.8(9) . . ? O4 C29 C28 121.7(9) . . ? C31 C29 C28 118.5(8) . . ? N5 C28 C27 122.9(9) . . ? N5 C28 C29 118.9(8) . . ? C27 C28 C29 118.1(8) . . ? C26 C27 C28 119.1(9) . . ? C26 C27 H27A 120.5 . . ? C28 C27 H27A 120.5 . . ? C27 C26 C25 118.6(9) . . ? C27 C26 H26A 120.7 . . ? C25 C26 H26A 120.7 . . ? C26 C25 C24 118.4(10) . . ? C26 C25 H25A 120.8 . . ? C24 C25 H25A 120.8 . . ? N5 C24 C25 123.1(8) . . ? N5 C24 C23 119.2(7) . . ? C25 C24 C23 117.6(9) . . ? O3 C23 C24 120.4(8) . . ? O3 C23 C21 119.5(8) . . ? C24 C23 C21 120.1(8) . . ? N4 C22 C21 123.4(8) . . ? N4 C22 H22A 118.3 . . ? C21 C22 H22A 118.3 . . ? C20 C21 C22 118.1(8) . . ? C20 C21 C23 123.7(8) . . ? C22 C21 C23 118.2(8) . . ? C21 C20 C19 119.6(8) . . ? C21 C20 H20A 120.2 . . ? C19 C20 H20A 120.2 . . ? C18 C19 C20 118.5(9) . . ? C18 C19 H19A 120.8 . . ? C20 C19 H19A 120.8 . . ? N4 C18 C19 122.7(8) . . ? N4 C18 H18A 118.7 . . ? C19 C18 H18A 118.7 . . ? O6 S1 O7 111.2(5) . . ? O6 S1 O5 109.0(5) . . ? O7 S1 O5 106.5(5) . . ? O6 S1 O8 112.0(4) . . ? O7 S1 O8 108.8(4) . . ? O5 S1 O8 109.2(4) . . ? S1 O7 Cd1 167.7(4) . 2_645 ? S1 O8 Cd1 128.1(4) . . ? Cd1 O4W H4WA 83.3 . . ? Cd1 O4W H4WB 144.2 . . ? H4WA O4W H4WB 124.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Cd1 N1 C5 158.1(6) 2_655 . . . ? O8 Cd1 N1 C5 69.6(6) . . . . ? O4W Cd1 N1 C5 -21.8(6) . . . . ? N3 Cd1 N1 C5 -107.9(6) . . . . ? N4 Cd1 N1 C5 -165.7(12) . . . . ? O7 Cd1 N1 C1 -30.8(5) 2_655 . . . ? O8 Cd1 N1 C1 -119.3(5) . . . . ? O4W Cd1 N1 C1 149.3(5) . . . . ? N3 Cd1 N1 C1 63.2(5) . . . . ? N4 Cd1 N1 C1 5.4(17) . . . . ? O7 Cd1 N3 C17 24.7(6) 2_655 . . . ? O8 Cd1 N3 C17 178(48) . . . . ? O4W Cd1 N3 C17 -155.7(6) . . . . ? N4 Cd1 N3 C17 110.4(5) . . . . ? N1 Cd1 N3 C17 -62.3(5) . . . . ? O7 Cd1 N3 C13 -164.2(7) 2_655 . . . ? O8 Cd1 N3 C13 -11(5) . . . . ? O4W Cd1 N3 C13 15.3(7) . . . . ? N4 Cd1 N3 C13 -78.6(7) . . . . ? N1 Cd1 N3 C13 108.7(7) . . . . ? O7 Cd1 N4 C22 -179.4(6) 2_655 . . . ? O8 Cd1 N4 C22 -90.6(6) . . . . ? O4W Cd1 N4 C22 0.5(6) . . . . ? N3 Cd1 N4 C22 86.7(6) . . . . ? N1 Cd1 N4 C22 144.4(13) . . . . ? O7 Cd1 N4 C18 -1.1(6) 2_655 . . . ? O8 Cd1 N4 C18 87.7(6) . . . . ? O4W Cd1 N4 C18 178.8(6) . . . . ? N3 Cd1 N4 C18 -95.0(6) . . . . ? N1 Cd1 N4 C18 -37.3(17) . . . . ? C5 N1 C1 C2 0.8(11) . . . . ? Cd1 N1 C1 C2 -170.9(6) . . . . ? N1 C1 C2 C3 -1.3(11) . . . . ? N1 C1 C2 C6 178.3(7) . . . . ? C1 C2 C3 C4 0.2(12) . . . . ? C6 C2 C3 C4 -179.4(8) . . . . ? C2 C3 C4 C5 1.2(13) . . . . ? C1 N1 C5 C4 0.7(12) . . . . ? Cd1 N1 C5 C4 171.7(6) . . . . ? C3 C4 C5 N1 -1.7(13) . . . . ? C3 C2 C6 O1 -35.2(12) . . . . ? C1 C2 C6 O1 145.2(8) . . . . ? C3 C2 C6 C7 145.8(8) . . . . ? C1 C2 C6 C7 -33.8(11) . . . . ? C11 N2 C7 C8 0.3(11) . . . . ? C11 N2 C7 C6 -176.8(7) . . . . ? O1 C6 C7 N2 156.1(7) . . . . ? C2 C6 C7 N2 -24.9(11) . . . . ? O1 C6 C7 C8 -21.1(13) . . . . ? C2 C6 C7 C8 157.9(8) . . . . ? N2 C7 C8 C9 1.4(13) . . . . ? C6 C7 C8 C9 178.4(8) . . . . ? C7 C8 C9 C10 -2.0(14) . . . . ? C8 C9 C10 C11 1.0(14) . . . . ? C7 N2 C11 C10 -1.3(11) . . . . ? C7 N2 C11 C12 176.9(6) . . . . ? C9 C10 C11 N2 0.6(13) . . . . ? C9 C10 C11 C12 -177.5(8) . . . . ? N2 C11 C12 O2 -158.4(8) . . . . ? C10 C11 C12 O2 19.8(12) . . . . ? N2 C11 C12 C16 22.4(10) . . . . ? C10 C11 C12 C16 -159.4(8) . . . . ? C17 N3 C13 C14 -0.2(12) . . . . ? Cd1 N3 C13 C14 -171.3(6) . . . . ? N3 C13 C14 C15 1.6(13) . . . . ? C13 C14 C15 C16 -1.6(13) . . . . ? C14 C15 C16 C17 0.2(12) . . . . ? C14 C15 C16 C12 -176.5(8) . . . . ? O2 C12 C16 C15 35.4(12) . . . . ? C11 C12 C16 C15 -145.4(8) . . . . ? O2 C12 C16 C17 -141.3(8) . . . . ? C11 C12 C16 C17 37.9(10) . . . . ? C13 N3 C17 C16 -1.2(11) . . . . ? Cd1 N3 C17 C16 170.5(5) . . . . ? C15 C16 C17 N3 1.3(11) . . . . ? C12 C16 C17 N3 178.1(7) . . . . ? C30 N6 C34 C33 0.0 . . . . ? N6 C34 C33 C32 0.0 . . . . ? C34 C33 C32 C31 0.0 . . . . ? C33 C32 C31 C30 0.0 . . . . ? C33 C32 C31 C29 -178.4(7) . . . . ? C32 C31 C30 N6 0.0 . . . . ? C29 C31 C30 N6 178.5(6) . . . . ? C34 N6 C30 C31 0.0 . . . . ? C32 C31 C29 O4 134.2(7) . . . . ? C30 C31 C29 O4 -44.2(9) . . . . ? C32 C31 C29 C28 -47.3(9) . . . . ? C30 C31 C29 C28 134.2(6) . . . . ? C24 N5 C28 C27 0.2(12) . . . . ? C24 N5 C28 C29 -174.8(8) . . . . ? O4 C29 C28 N5 166.9(8) . . . . ? C31 C29 C28 N5 -11.5(11) . . . . ? O4 C29 C28 C27 -8.3(13) . . . . ? C31 C29 C28 C27 173.2(8) . . . . ? N5 C28 C27 C26 -0.6(15) . . . . ? C29 C28 C27 C26 174.5(9) . . . . ? C28 C27 C26 C25 0.9(16) . . . . ? C27 C26 C25 C24 -0.8(16) . . . . ? C28 N5 C24 C25 -0.1(13) . . . . ? C28 N5 C24 C23 175.4(7) . . . . ? C26 C25 C24 N5 0.4(14) . . . . ? C26 C25 C24 C23 -175.2(9) . . . . ? N5 C24 C23 O3 -166.7(9) . . . . ? C25 C24 C23 O3 9.1(13) . . . . ? N5 C24 C23 C21 13.3(12) . . . . ? C25 C24 C23 C21 -170.9(8) . . . . ? C18 N4 C22 C21 2.4(11) . . . . ? Cd1 N4 C22 C21 -179.3(6) . . . . ? N4 C22 C21 C20 -1.5(12) . . . . ? N4 C22 C21 C23 178.1(7) . . . . ? O3 C23 C21 C20 -140.5(10) . . . . ? C24 C23 C21 C20 39.5(12) . . . . ? O3 C23 C21 C22 39.9(12) . . . . ? C24 C23 C21 C22 -140.0(8) . . . . ? C22 C21 C20 C19 -1.5(12) . . . . ? C23 C21 C20 C19 179.0(8) . . . . ? C21 C20 C19 C18 3.3(13) . . . . ? C22 N4 C18 C19 -0.4(12) . . . . ? Cd1 N4 C18 C19 -178.8(6) . . . . ? C20 C19 C18 N4 -2.5(12) . . . . ? O6 S1 O7 Cd1 40(3) . . . 2_645 ? O5 S1 O7 Cd1 -79(2) . . . 2_645 ? O8 S1 O7 Cd1 163(2) . . . 2_645 ? O6 S1 O8 Cd1 -148.7(5) . . . . ? O7 S1 O8 Cd1 88.0(5) . . . . ? O5 S1 O8 Cd1 -27.9(6) . . . . ? O7 Cd1 O8 S1 169.1(5) 2_655 . . . ? O4W Cd1 O8 S1 -10.4(5) . . . . ? N3 Cd1 O8 S1 16(5) . . . . ? N4 Cd1 O8 S1 83.4(4) . . . . ? N1 Cd1 O8 S1 -103.7(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.775 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.122 #####################################end################################ data_complex7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H17 Cd N3 O6' _chemical_formula_weight 519.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 8.8794(17) _cell_length_b 10.993(2) _cell_length_c 12.0665(17) _cell_angle_alpha 90.00 _cell_angle_beta 121.531(10) _cell_angle_gamma 90.00 _cell_volume 1003.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 1.133 _exptl_absorpt_correction_type Multi-SCAN _exptl_absorpt_correction_T_min 0.731263 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5200 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1775 _reflns_number_gt 1717 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker 2007)' _computing_cell_refinement 'APEX2 and SAINT (Bruker 2007)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.8299P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment Constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1775 _refine_ls_number_parameters 143 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.43943(2) 0.7500 0.02930(12) Uani 1 2 d S . . O1 O 0.2139(3) -0.0455(2) 0.5847(2) 0.0476(6) Uani 1 1 d . . . O2 O 0.7076(3) 0.5843(2) 0.8887(2) 0.0438(5) Uani 1 1 d . . . O3 O 0.7516(3) 0.4902(2) 0.7490(2) 0.0478(5) Uani 1 1 d . . . N1 N 0.4311(3) 0.2900(2) 0.5930(2) 0.0312(5) Uani 1 1 d . . . N2 N 0.0000 -0.0155(3) 0.2500 0.0261(6) Uani 1 2 d S . . C1 C 0.4795(4) 0.3089(3) 0.5059(3) 0.0345(6) Uani 1 1 d . . . H1A H 0.5453 0.3778 0.5142 0.041 Uiso 1 1 calc R . . C2 C 0.4354(4) 0.2299(3) 0.4049(3) 0.0363(6) Uani 1 1 d . . . H2A H 0.4707 0.2458 0.3461 0.044 Uiso 1 1 calc R . . C3 C 0.3384(4) 0.1271(3) 0.3917(2) 0.0317(6) Uani 1 1 d . . . H3A H 0.3056 0.0735 0.3230 0.038 Uiso 1 1 calc R . . C4 C 0.2903(3) 0.1048(2) 0.4830(2) 0.0266(5) Uani 1 1 d . . . C5 C 0.3393(3) 0.1893(2) 0.5811(2) 0.0296(5) Uani 1 1 d . . . H5A H 0.3067 0.1754 0.6418 0.036 Uiso 1 1 calc R . . C6 C 0.1985(3) -0.0089(2) 0.4840(2) 0.0298(5) Uani 1 1 d . . . C7 C 0.0926(3) -0.0799(2) 0.3603(2) 0.0272(5) Uani 1 1 d . . . C8 C 0.0942(4) -0.2064(2) 0.3651(3) 0.0335(6) Uani 1 1 d . . . H8A H 0.1574 -0.2471 0.4441 0.040 Uiso 1 1 calc R . . C9 C 0.0000 -0.2700(4) 0.2500 0.0387(9) Uani 1 2 d S . . H9A H 0.0000 -0.3546 0.2500 0.046 Uiso 1 2 calc SR . . C10 C 0.7992(4) 0.5648(2) 0.8402(3) 0.0354(6) Uani 1 1 d . . . C11 C 0.9698(4) 0.6336(4) 0.8906(3) 0.0534(8) Uani 1 1 d . . . H11A H 0.9454 0.7118 0.8492 0.064 Uiso 1 1 calc R . . H11B H 1.0464 0.5886 0.8717 0.064 Uiso 1 1 calc R . . H11C H 1.0263 0.6442 0.9829 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03162(18) 0.02535(17) 0.02895(17) 0.000 0.01446(13) 0.000 O1 0.0658(15) 0.0489(13) 0.0263(10) 0.0037(9) 0.0228(11) -0.0125(11) O2 0.0396(11) 0.0506(12) 0.0454(12) -0.0158(10) 0.0252(10) -0.0078(10) O3 0.0428(12) 0.0505(13) 0.0540(13) -0.0209(11) 0.0282(10) -0.0093(10) N1 0.0337(12) 0.0303(12) 0.0283(11) -0.0023(9) 0.0153(10) -0.0017(9) N2 0.0286(15) 0.0248(15) 0.0223(14) 0.000 0.0114(12) 0.000 C1 0.0344(14) 0.0317(14) 0.0345(14) 0.0011(12) 0.0161(12) -0.0032(11) C2 0.0420(15) 0.0431(16) 0.0298(13) 0.0014(12) 0.0230(12) -0.0040(12) C3 0.0355(14) 0.0353(14) 0.0238(12) -0.0047(11) 0.0152(11) -0.0023(11) C4 0.0250(12) 0.0289(13) 0.0207(11) 0.0024(10) 0.0084(10) 0.0021(10) C5 0.0310(13) 0.0356(14) 0.0220(11) 0.0025(11) 0.0137(10) 0.0022(11) C6 0.0307(13) 0.0320(14) 0.0232(12) 0.0041(11) 0.0116(11) 0.0017(11) C7 0.0264(12) 0.0282(13) 0.0258(13) 0.0007(10) 0.0129(11) -0.0016(10) C8 0.0336(14) 0.0280(13) 0.0355(14) 0.0085(11) 0.0156(12) 0.0030(11) C9 0.043(2) 0.0211(18) 0.050(2) 0.000 0.023(2) 0.000 C10 0.0313(14) 0.0356(16) 0.0344(14) -0.0003(11) 0.0138(12) 0.0010(11) C11 0.0378(17) 0.066(2) 0.0538(19) -0.0124(17) 0.0222(15) -0.0129(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.309(2) 2_656 ? Cd1 O3 2.309(2) . ? Cd1 N1 2.335(2) . ? Cd1 N1 2.335(2) 2_656 ? Cd1 O2 2.347(2) . ? Cd1 O2 2.347(2) 2_656 ? Cd1 C10 2.668(3) . ? Cd1 C10 2.668(3) 2_656 ? O1 C6 1.218(3) . ? O2 C10 1.245(4) . ? O3 C10 1.256(4) . ? N1 C5 1.337(3) . ? N1 C1 1.343(3) . ? N2 C7 1.343(3) 2 ? N2 C7 1.343(3) . ? C1 C2 1.375(4) . ? C1 H1A 0.9300 . ? C2 C3 1.379(4) . ? C2 H2A 0.9300 . ? C3 C4 1.396(4) . ? C3 H3A 0.9300 . ? C4 C5 1.385(4) . ? C4 C6 1.495(4) . ? C5 H5A 0.9300 . ? C6 C7 1.501(4) . ? C7 C8 1.392(4) . ? C8 C9 1.379(3) . ? C8 H8A 0.9300 . ? C9 C8 1.379(3) 2 ? C9 H9A 0.9300 . ? C10 C11 1.508(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cd1 O3 152.02(12) 2_656 . ? O3 Cd1 N1 109.32(8) 2_656 . ? O3 Cd1 N1 90.53(8) . . ? O3 Cd1 N1 90.53(8) 2_656 2_656 ? O3 Cd1 N1 109.32(8) . 2_656 ? N1 Cd1 N1 90.58(11) . 2_656 ? O3 Cd1 O2 103.49(8) 2_656 . ? O3 Cd1 O2 55.86(7) . . ? N1 Cd1 O2 146.20(7) . . ? N1 Cd1 O2 97.11(8) 2_656 . ? O3 Cd1 O2 55.86(7) 2_656 2_656 ? O3 Cd1 O2 103.49(8) . 2_656 ? N1 Cd1 O2 97.11(8) . 2_656 ? N1 Cd1 O2 146.20(7) 2_656 2_656 ? O2 Cd1 O2 94.54(12) . 2_656 ? O3 Cd1 C10 129.25(9) 2_656 . ? O3 Cd1 C10 28.06(8) . . ? N1 Cd1 C10 118.49(8) . . ? N1 Cd1 C10 104.48(8) 2_656 . ? O2 Cd1 C10 27.80(8) . . ? O2 Cd1 C10 100.57(8) 2_656 . ? O3 Cd1 C10 28.06(8) 2_656 2_656 ? O3 Cd1 C10 129.25(9) . 2_656 ? N1 Cd1 C10 104.48(8) . 2_656 ? N1 Cd1 C10 118.49(8) 2_656 2_656 ? O2 Cd1 C10 100.57(8) . 2_656 ? O2 Cd1 C10 27.80(8) 2_656 2_656 ? C10 Cd1 C10 117.78(12) . 2_656 ? C10 O2 Cd1 90.61(17) . . ? C10 O3 Cd1 92.09(18) . . ? C5 N1 C1 118.1(2) . . ? C5 N1 Cd1 123.72(17) . . ? C1 N1 Cd1 118.10(18) . . ? C7 N2 C7 116.4(3) 2 . ? N1 C1 C2 122.4(3) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C1 C2 C3 119.4(2) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? C2 C3 C4 118.9(2) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C5 C4 C3 117.9(2) . . ? C5 C4 C6 118.9(2) . . ? C3 C4 C6 123.1(2) . . ? N1 C5 C4 123.3(2) . . ? N1 C5 H5A 118.4 . . ? C4 C5 H5A 118.4 . . ? O1 C6 C4 120.5(2) . . ? O1 C6 C7 120.3(2) . . ? C4 C6 C7 119.2(2) . . ? N2 C7 C8 123.7(2) . . ? N2 C7 C6 116.9(2) . . ? C8 C7 C6 119.4(2) . . ? C9 C8 C7 118.5(3) . . ? C9 C8 H8A 120.7 . . ? C7 C8 H8A 120.7 . . ? C8 C9 C8 119.1(3) . 2 ? C8 C9 H9A 120.5 . . ? C8 C9 H9A 120.5 2 . ? O2 C10 O3 121.4(3) . . ? O2 C10 C11 119.4(3) . . ? O3 C10 C11 119.2(3) . . ? O2 C10 Cd1 61.59(15) . . ? O3 C10 Cd1 59.85(15) . . ? C11 C10 Cd1 178.9(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Cd1 O2 C10 -160.06(17) 2_656 . . . ? O3 Cd1 O2 C10 -0.88(17) . . . . ? N1 Cd1 O2 C10 5.9(3) . . . . ? N1 Cd1 O2 C10 107.68(18) 2_656 . . . ? O2 Cd1 O2 C10 -104.11(19) 2_656 . . . ? C10 Cd1 O2 C10 -131.51(17) 2_656 . . . ? O3 Cd1 O3 C10 48.35(17) 2_656 . . . ? N1 Cd1 O3 C10 -175.37(18) . . . . ? N1 Cd1 O3 C10 -84.57(19) 2_656 . . . ? O2 Cd1 O3 C10 0.88(16) . . . . ? O2 Cd1 O3 C10 87.19(19) 2_656 . . . ? C10 Cd1 O3 C10 75.3(2) 2_656 . . . ? O3 Cd1 N1 C5 -48.4(2) 2_656 . . . ? O3 Cd1 N1 C5 151.7(2) . . . . ? N1 Cd1 N1 C5 42.33(18) 2_656 . . . ? O2 Cd1 N1 C5 146.07(19) . . . . ? O2 Cd1 N1 C5 -104.7(2) 2_656 . . . ? C10 Cd1 N1 C5 149.2(2) . . . . ? C10 Cd1 N1 C5 -77.4(2) 2_656 . . . ? O3 Cd1 N1 C1 128.42(19) 2_656 . . . ? O3 Cd1 N1 C1 -31.5(2) . . . . ? N1 Cd1 N1 C1 -140.8(2) 2_656 . . . ? O2 Cd1 N1 C1 -37.1(3) . . . . ? O2 Cd1 N1 C1 72.2(2) 2_656 . . . ? C10 Cd1 N1 C1 -34.0(2) . . . . ? C10 Cd1 N1 C1 99.5(2) 2_656 . . . ? C5 N1 C1 C2 1.2(4) . . . . ? Cd1 N1 C1 C2 -175.9(2) . . . . ? N1 C1 C2 C3 -0.2(4) . . . . ? C1 C2 C3 C4 -1.2(4) . . . . ? C2 C3 C4 C5 1.5(4) . . . . ? C2 C3 C4 C6 -174.7(2) . . . . ? C1 N1 C5 C4 -0.8(4) . . . . ? Cd1 N1 C5 C4 176.10(18) . . . . ? C3 C4 C5 N1 -0.6(4) . . . . ? C6 C4 C5 N1 175.8(2) . . . . ? C5 C4 C6 O1 -22.5(4) . . . . ? C3 C4 C6 O1 153.7(3) . . . . ? C5 C4 C6 C7 159.8(2) . . . . ? C3 C4 C6 C7 -24.0(4) . . . . ? C7 N2 C7 C8 -1.05(19) 2 . . . ? C7 N2 C7 C6 179.2(3) 2 . . . ? O1 C6 C7 N2 144.3(3) . . . . ? C4 C6 C7 N2 -37.9(3) . . . . ? O1 C6 C7 C8 -35.4(4) . . . . ? C4 C6 C7 C8 142.3(3) . . . . ? N2 C7 C8 C9 2.1(4) . . . . ? C6 C7 C8 C9 -178.2(2) . . . . ? C7 C8 C9 C8 -0.95(17) . . . 2 ? Cd1 O2 C10 O3 1.6(3) . . . . ? Cd1 O2 C10 C11 -179.4(3) . . . . ? Cd1 O3 C10 O2 -1.6(3) . . . . ? Cd1 O3 C10 C11 179.3(3) . . . . ? O3 Cd1 C10 O2 25.4(2) 2_656 . . . ? O3 Cd1 C10 O2 178.4(3) . . . . ? N1 Cd1 C10 O2 -176.29(16) . . . . ? N1 Cd1 C10 O2 -77.55(18) 2_656 . . . ? O2 Cd1 C10 O2 79.6(2) 2_656 . . . ? C10 Cd1 C10 O2 56.31(16) 2_656 . . . ? O3 Cd1 C10 O3 -153.09(15) 2_656 . . . ? N1 Cd1 C10 O3 5.3(2) . . . . ? N1 Cd1 C10 O3 104.01(18) 2_656 . . . ? O2 Cd1 C10 O3 -178.4(3) . . . . ? O2 Cd1 C10 O3 -98.88(18) 2_656 . . . ? C10 Cd1 C10 O3 -122.13(19) 2_656 . . . ? O3 Cd1 C10 C11 176(100) 2_656 . . . ? O3 Cd1 C10 C11 -31(12) . . . . ? N1 Cd1 C10 C11 -26(12) . . . . ? N1 Cd1 C10 C11 73(12) 2_656 . . . ? O2 Cd1 C10 C11 150(12) . . . . ? O2 Cd1 C10 C11 -130(12) 2_656 . . . ? C10 Cd1 C10 C11 -153(12) 2_656 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.670 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.071 #######################################end############################# data_complex8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H17 N3 O6 Zn' _chemical_formula_weight 472.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 8.7188(3) _cell_length_b 10.9954(3) _cell_length_c 12.0144(3) _cell_angle_alpha 90.00 _cell_angle_beta 121.556(2) _cell_angle_gamma 90.00 _cell_volume 981.47(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 484 _exptl_absorpt_coefficient_mu 1.297 _exptl_absorpt_correction_type Multi-SCAN _exptl_absorpt_correction_T_min 0.800023 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10958 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.0112 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1741 _reflns_number_gt 1655 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker 2007)' _computing_cell_refinement 'APEX2 and SAINT (Bruker 2007)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.4553P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1741 _refine_ls_number_parameters 143 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5000 0.08082(3) 0.7500 0.03704(13) Uani 1 2 d S . . O1 O 0.2154(3) 0.54932(16) 0.58580(15) 0.0570(4) Uani 1 1 d . . . O2 O 0.7271(2) 0.02791(15) 0.75652(16) 0.0519(4) Uani 1 1 d . . . O3 O 0.6921(2) -0.07556(15) 0.89537(18) 0.0573(4) Uani 1 1 d . . . N1 N 0.4225(2) 0.20829(15) 0.59798(15) 0.0361(4) Uani 1 1 d . . . N2 N 0.0000 0.51740(19) 0.2500 0.0328(5) Uani 1 2 d S . . C1 C 0.4691(3) 0.18513(18) 0.50996(19) 0.0410(5) Uani 1 1 d . . . H1A H 0.5327 0.1143 0.5186 0.049 Uiso 1 1 calc R . . C2 C 0.4266(3) 0.2619(2) 0.40763(19) 0.0441(5) Uani 1 1 d . . . H2A H 0.4607 0.2429 0.3482 0.053 Uiso 1 1 calc R . . C3 C 0.3331(3) 0.36747(19) 0.39367(18) 0.0392(4) Uani 1 1 d . . . H3A H 0.3022 0.4201 0.3244 0.047 Uiso 1 1 calc R . . C4 C 0.2855(2) 0.39395(17) 0.48509(17) 0.0332(4) Uani 1 1 d . . . C5 C 0.3330(3) 0.31102(18) 0.58486(17) 0.0354(4) Uani 1 1 d . . . H5A H 0.3008 0.3278 0.6458 0.043 Uiso 1 1 calc R . . C6 C 0.1978(3) 0.51031(18) 0.48551(18) 0.0370(4) Uani 1 1 d . . . C7 C 0.0937(3) 0.58113(16) 0.36098(19) 0.0341(4) Uani 1 1 d . . . C8 C 0.0953(3) 0.70739(18) 0.3656(2) 0.0426(5) Uani 1 1 d . . . H8A H 0.1593 0.7481 0.4451 0.051 Uiso 1 1 calc R . . C9 C 0.0000 0.7713(3) 0.2500 0.0477(7) Uani 1 2 d S . . H9A H 0.0000 0.8559 0.2500 0.057 Uiso 1 2 calc SR . . C10 C 0.7782(3) -0.05245(19) 0.8432(2) 0.0416(5) Uani 1 1 d . . . C11 C 0.9490(4) -0.1209(3) 0.8829(3) 0.0645(7) Uani 1 1 d . . . H11A H 1.0070 -0.1431 0.9733 0.077 Uiso 1 1 calc R . . H11B H 1.0281 -0.0702 0.8699 0.077 Uiso 1 1 calc R . . H11C H 0.9208 -0.1930 0.8306 0.077 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0401(2) 0.0340(2) 0.0344(2) 0.000 0.01760(15) 0.000 O1 0.0782(12) 0.0551(9) 0.0326(8) -0.0054(7) 0.0255(8) 0.0146(8) O2 0.0489(9) 0.0511(9) 0.0517(9) 0.0147(7) 0.0235(7) 0.0079(7) O3 0.0533(10) 0.0601(11) 0.0629(11) 0.0109(8) 0.0334(9) 0.0016(7) N1 0.0404(9) 0.0336(8) 0.0304(8) 0.0016(6) 0.0157(7) 0.0015(7) N2 0.0376(12) 0.0285(11) 0.0289(11) 0.000 0.0151(9) 0.000 C1 0.0457(11) 0.0373(10) 0.0376(10) -0.0010(8) 0.0201(9) 0.0066(9) C2 0.0509(12) 0.0503(12) 0.0349(10) 0.0013(9) 0.0252(9) 0.0095(10) C3 0.0434(11) 0.0437(11) 0.0287(9) 0.0047(8) 0.0175(8) 0.0049(9) C4 0.0320(9) 0.0343(9) 0.0262(9) -0.0018(7) 0.0103(7) -0.0009(7) C5 0.0383(10) 0.0388(10) 0.0274(9) -0.0010(7) 0.0159(8) 0.0003(8) C6 0.0393(10) 0.0375(10) 0.0295(9) -0.0040(8) 0.0146(8) -0.0003(8) C7 0.0352(10) 0.0322(10) 0.0322(10) -0.0031(7) 0.0158(8) 0.0007(7) C8 0.0443(11) 0.0337(10) 0.0443(11) -0.0091(8) 0.0193(9) -0.0025(8) C9 0.0536(18) 0.0266(14) 0.0600(19) 0.000 0.0277(15) 0.000 C10 0.0381(11) 0.0392(10) 0.0407(11) 0.0003(9) 0.0159(9) -0.0019(8) C11 0.0523(14) 0.0692(16) 0.0675(16) 0.0128(14) 0.0282(13) 0.0160(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 2.0253(16) 2_656 ? Zn1 O2 2.0253(16) . ? Zn1 N1 2.1131(16) 2_656 ? Zn1 N1 2.1131(16) . ? Zn1 O3 2.3979(17) 2_656 ? Zn1 O3 2.3979(17) . ? Zn1 C10 2.538(2) 2_656 ? Zn1 C10 2.538(2) . ? O1 C6 1.211(2) . ? O2 C10 1.256(3) . ? O3 C10 1.230(3) . ? N1 C5 1.335(3) . ? N1 C1 1.341(3) . ? N2 C7 1.340(2) . ? N2 C7 1.340(2) 2 ? C1 C2 1.373(3) . ? C1 H1A 0.9300 . ? C2 C3 1.377(3) . ? C2 H2A 0.9300 . ? C3 C4 1.393(3) . ? C3 H3A 0.9300 . ? C4 C5 1.386(3) . ? C4 C6 1.491(3) . ? C5 H5A 0.9300 . ? C6 C7 1.499(3) . ? C7 C8 1.389(3) . ? C8 C9 1.381(3) . ? C8 H8A 0.9300 . ? C9 C8 1.381(3) 2 ? C9 H9A 0.9300 . ? C10 C11 1.506(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O2 146.61(9) 2_656 . ? O2 Zn1 N1 95.04(6) 2_656 2_656 ? O2 Zn1 N1 107.05(7) . 2_656 ? O2 Zn1 N1 107.05(7) 2_656 . ? O2 Zn1 N1 95.04(6) . . ? N1 Zn1 N1 96.90(9) 2_656 . ? O2 Zn1 O3 57.99(6) 2_656 2_656 ? O2 Zn1 O3 96.78(7) . 2_656 ? N1 Zn1 O3 152.96(6) 2_656 2_656 ? N1 Zn1 O3 93.47(6) . 2_656 ? O2 Zn1 O3 96.78(6) 2_656 . ? O2 Zn1 O3 57.99(6) . . ? N1 Zn1 O3 93.47(6) 2_656 . ? N1 Zn1 O3 152.96(6) . . ? O3 Zn1 O3 88.37(9) 2_656 . ? O2 Zn1 C10 29.30(7) 2_656 2_656 ? O2 Zn1 C10 122.71(7) . 2_656 ? N1 Zn1 C10 124.31(7) 2_656 2_656 ? N1 Zn1 C10 101.66(7) . 2_656 ? O3 Zn1 C10 28.69(6) 2_656 2_656 ? O3 Zn1 C10 92.83(6) . 2_656 ? O2 Zn1 C10 122.71(7) 2_656 . ? O2 Zn1 C10 29.30(7) . . ? N1 Zn1 C10 101.66(7) 2_656 . ? N1 Zn1 C10 124.31(7) . . ? O3 Zn1 C10 92.83(6) 2_656 . ? O3 Zn1 C10 28.69(6) . . ? C10 Zn1 C10 109.48(9) 2_656 . ? C10 O2 Zn1 98.61(14) . . ? C10 O3 Zn1 82.00(13) . . ? C5 N1 C1 117.87(16) . . ? C5 N1 Zn1 124.47(13) . . ? C1 N1 Zn1 117.64(13) . . ? C7 N2 C7 117.0(2) . 2 ? N1 C1 C2 122.55(18) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C1 C2 C3 119.52(19) . . ? C1 C2 H2A 120.2 . . ? C3 C2 H2A 120.2 . . ? C2 C3 C4 118.81(18) . . ? C2 C3 H3A 120.6 . . ? C4 C3 H3A 120.6 . . ? C5 C4 C3 117.84(18) . . ? C5 C4 C6 118.90(17) . . ? C3 C4 C6 123.12(17) . . ? N1 C5 C4 123.41(17) . . ? N1 C5 H5A 118.3 . . ? C4 C5 H5A 118.3 . . ? O1 C6 C4 120.60(18) . . ? O1 C6 C7 120.28(18) . . ? C4 C6 C7 119.08(16) . . ? N2 C7 C8 123.41(18) . . ? N2 C7 C6 117.18(16) . . ? C8 C7 C6 119.40(17) . . ? C9 C8 C7 118.7(2) . . ? C9 C8 H8A 120.7 . . ? C7 C8 H8A 120.7 . . ? C8 C9 C8 118.8(3) 2 . ? C8 C9 H9A 120.6 2 . ? C8 C9 H9A 120.6 . . ? O3 C10 O2 121.4(2) . . ? O3 C10 C11 120.1(2) . . ? O2 C10 C11 118.5(2) . . ? O3 C10 Zn1 69.31(13) . . ? O2 C10 Zn1 52.09(11) . . ? C11 C10 Zn1 170.57(18) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Zn1 O2 C10 -45.80(12) 2_656 . . . ? N1 Zn1 O2 C10 83.42(14) 2_656 . . . ? N1 Zn1 O2 C10 -177.77(13) . . . . ? O3 Zn1 O2 C10 -83.66(14) 2_656 . . . ? O3 Zn1 O2 C10 0.14(13) . . . . ? C10 Zn1 O2 C10 -70.45(18) 2_656 . . . ? O2 Zn1 O3 C10 156.39(13) 2_656 . . . ? O2 Zn1 O3 C10 -0.14(13) . . . . ? N1 Zn1 O3 C10 -108.11(14) 2_656 . . . ? N1 Zn1 O3 C10 4.4(2) . . . . ? O3 Zn1 O3 C10 98.90(14) 2_656 . . . ? C10 Zn1 O3 C10 127.25(13) 2_656 . . . ? O2 Zn1 N1 C5 57.19(16) 2_656 . . . ? O2 Zn1 N1 C5 -148.15(16) . . . . ? N1 Zn1 N1 C5 -40.26(13) 2_656 . . . ? O3 Zn1 N1 C5 114.72(16) 2_656 . . . ? O3 Zn1 N1 C5 -152.05(15) . . . . ? C10 Zn1 N1 C5 86.95(16) 2_656 . . . ? C10 Zn1 N1 C5 -149.47(15) . . . . ? O2 Zn1 N1 C1 -123.91(15) 2_656 . . . ? O2 Zn1 N1 C1 30.75(16) . . . . ? N1 Zn1 N1 C1 138.64(17) 2_656 . . . ? O3 Zn1 N1 C1 -66.38(15) 2_656 . . . ? O3 Zn1 N1 C1 26.9(2) . . . . ? C10 Zn1 N1 C1 -94.14(15) 2_656 . . . ? C10 Zn1 N1 C1 29.43(17) . . . . ? C5 N1 C1 C2 -0.7(3) . . . . ? Zn1 N1 C1 C2 -179.68(16) . . . . ? N1 C1 C2 C3 0.2(3) . . . . ? C1 C2 C3 C4 0.6(3) . . . . ? C2 C3 C4 C5 -0.9(3) . . . . ? C2 C3 C4 C6 174.75(19) . . . . ? C1 N1 C5 C4 0.3(3) . . . . ? Zn1 N1 C5 C4 179.22(14) . . . . ? C3 C4 C5 N1 0.5(3) . . . . ? C6 C4 C5 N1 -175.37(18) . . . . ? C5 C4 C6 O1 22.0(3) . . . . ? C3 C4 C6 O1 -153.6(2) . . . . ? C5 C4 C6 C7 -160.45(18) . . . . ? C3 C4 C6 C7 23.9(3) . . . . ? C7 N2 C7 C8 1.00(15) 2 . . . ? C7 N2 C7 C6 179.6(2) 2 . . . ? O1 C6 C7 N2 -146.23(19) . . . . ? C4 C6 C7 N2 36.2(3) . . . . ? O1 C6 C7 C8 32.4(3) . . . . ? C4 C6 C7 C8 -145.1(2) . . . . ? N2 C7 C8 C9 -2.0(3) . . . . ? C6 C7 C8 C9 179.45(15) . . . . ? C7 C8 C9 C8 0.92(14) . . . 2 ? Zn1 O3 C10 O2 0.2(2) . . . . ? Zn1 O3 C10 C11 -179.8(2) . . . . ? Zn1 O2 C10 O3 -0.3(2) . . . . ? Zn1 O2 C10 C11 179.75(19) . . . . ? O2 Zn1 C10 O3 -28.21(16) 2_656 . . . ? O2 Zn1 C10 O3 179.8(2) . . . . ? N1 Zn1 C10 O3 75.63(14) 2_656 . . . ? N1 Zn1 C10 O3 -177.56(12) . . . . ? O3 Zn1 C10 O3 -81.41(16) 2_656 . . . ? C10 Zn1 C10 O3 -57.49(12) 2_656 . . . ? O2 Zn1 C10 O2 152.04(11) 2_656 . . . ? N1 Zn1 C10 O2 -104.13(14) 2_656 . . . ? N1 Zn1 C10 O2 2.69(16) . . . . ? O3 Zn1 C10 O2 98.84(14) 2_656 . . . ? O3 Zn1 C10 O2 -179.8(2) . . . . ? C10 Zn1 C10 O2 122.75(15) 2_656 . . . ? O2 Zn1 C10 C11 150.7(11) 2_656 . . . ? O2 Zn1 C10 C11 -1.4(10) . . . . ? N1 Zn1 C10 C11 -105.5(11) 2_656 . . . ? N1 Zn1 C10 C11 1.3(11) . . . . ? O3 Zn1 C10 C11 97.5(11) 2_656 . . . ? O3 Zn1 C10 C11 178.9(11) . . . . ? C10 Zn1 C10 C11 121.4(11) 2_656 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.287 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.047 #############################end###################### data_complex9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H17 Hg N3 O6' _chemical_formula_weight 607.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 8.9228(19) _cell_length_b 10.996(2) _cell_length_c 12.0653(18) _cell_angle_alpha 90.00 _cell_angle_beta 121.556(11) _cell_angle_gamma 90.00 _cell_volume 1008.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description stick _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.002 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 7.674 _exptl_absorpt_correction_type Multi-SCAN _exptl_absorpt_correction_T_min 0.394392 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5280 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1781 _reflns_number_gt 1474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELTXL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1781 _refine_ls_number_parameters 143 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg1 Hg 0.5000 0.05958(4) 0.7500 0.03926(18) Uani 1 2 d S . . O1 O 0.2142(9) 0.5422(5) 0.5835(5) 0.0579(16) Uani 1 1 d . . . O2 O 0.7576(8) 0.0063(6) 0.7499(6) 0.0658(18) Uani 1 1 d . . . O3 O 0.7174(8) -0.0885(6) 0.8902(6) 0.0605(17) Uani 1 1 d . . . N1 N 0.4356(8) 0.2114(5) 0.5928(5) 0.0373(15) Uani 1 1 d . . . N2 N 0.0000 0.5135(7) 0.2500 0.0312(19) Uani 1 2 d S . . C1 C 0.4826(10) 0.1931(7) 0.5042(7) 0.0404(18) Uani 1 1 d . . . H1A H 0.5486 0.1245 0.5121 0.048 Uiso 1 1 calc R . . C2 C 0.4372(11) 0.2711(7) 0.4040(7) 0.0435(19) Uani 1 1 d . . . H2A H 0.4727 0.2563 0.3452 0.052 Uiso 1 1 calc R . . C3 C 0.3374(10) 0.3730(7) 0.3904(7) 0.0383(18) Uani 1 1 d . . . H3A H 0.3027 0.4264 0.3213 0.046 Uiso 1 1 calc R . . C4 C 0.2907(9) 0.3939(7) 0.4806(6) 0.0321(16) Uani 1 1 d . . . C5 C 0.3444(9) 0.3098(7) 0.5803(6) 0.0341(17) Uani 1 1 d . . . H5A H 0.3141 0.3240 0.6421 0.041 Uiso 1 1 calc R . . C6 C 0.1981(10) 0.5072(7) 0.4826(7) 0.0363(17) Uani 1 1 d . . . C7 C 0.0923(9) 0.5781(6) 0.3603(7) 0.0321(16) Uani 1 1 d . . . C8 C 0.0934(10) 0.7030(7) 0.3649(7) 0.0418(19) Uani 1 1 d . . . H8A H 0.1560 0.7435 0.4441 0.050 Uiso 1 1 calc R . . C9 C 0.0000 0.7673(10) 0.2500 0.049(3) Uani 1 2 d S . . H9A H 0.0000 0.8519 0.2500 0.058 Uiso 1 2 calc SR . . C10 C 0.8039(11) -0.0682(7) 0.8401(8) 0.0439(19) Uani 1 1 d . . . C11 C 0.9768(12) -0.1344(10) 0.8923(9) 0.068(3) Uani 1 1 d . . . H11A H 1.0361 -0.1396 0.9853 0.101 Uiso 1 1 calc R . . H11B H 1.0490 -0.0908 0.8685 0.101 Uiso 1 1 calc R . . H11C H 0.9548 -0.2149 0.8561 0.101 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Hg1 0.0441(3) 0.0315(3) 0.0400(3) 0.000 0.0205(2) 0.000 O1 0.083(5) 0.056(4) 0.034(3) -0.002(3) 0.030(3) 0.014(3) O2 0.045(4) 0.068(4) 0.076(4) 0.034(4) 0.025(4) 0.008(3) O3 0.050(4) 0.067(4) 0.065(4) 0.018(3) 0.030(4) 0.014(3) N1 0.038(4) 0.038(4) 0.031(3) 0.006(3) 0.014(3) 0.004(3) N2 0.043(5) 0.025(4) 0.032(5) 0.000 0.023(4) 0.000 C1 0.043(5) 0.040(4) 0.040(4) -0.007(4) 0.023(4) 0.002(4) C2 0.050(5) 0.052(5) 0.032(4) 0.003(4) 0.023(4) 0.006(4) C3 0.046(5) 0.045(5) 0.027(4) 0.000(3) 0.021(4) -0.004(4) C4 0.031(4) 0.035(4) 0.022(4) -0.004(3) 0.008(3) -0.007(3) C5 0.033(4) 0.045(5) 0.019(3) -0.005(3) 0.010(3) -0.004(4) C6 0.044(5) 0.035(4) 0.030(4) -0.003(3) 0.020(4) -0.001(4) C7 0.033(4) 0.033(4) 0.032(4) -0.006(3) 0.018(3) -0.001(3) C8 0.037(5) 0.040(5) 0.036(4) -0.011(4) 0.011(4) -0.004(4) C9 0.061(8) 0.024(6) 0.057(8) 0.000 0.027(7) 0.000 C10 0.039(5) 0.041(5) 0.043(5) 0.002(4) 0.015(4) -0.003(4) C11 0.054(6) 0.079(7) 0.071(6) 0.024(5) 0.034(5) 0.023(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg1 N1 2.361(6) 2_656 ? Hg1 N1 2.361(6) . ? Hg1 O2 2.373(6) 2_656 ? Hg1 O2 2.373(6) . ? Hg1 O3 2.417(6) 2_656 ? Hg1 O3 2.417(6) . ? Hg1 C10 2.725(8) 2_656 ? Hg1 C10 2.725(8) . ? O1 C6 1.211(8) . ? O2 C10 1.247(10) . ? O3 C10 1.223(10) . ? N1 C5 1.314(9) . ? N1 C1 1.352(9) . ? N2 C7 1.345(8) . ? N2 C7 1.345(8) 2 ? C1 C2 1.360(10) . ? C1 H1A 0.9300 . ? C2 C3 1.386(11) . ? C2 H2A 0.9300 . ? C3 C4 1.373(10) . ? C3 H3A 0.9300 . ? C4 C5 1.388(10) . ? C4 C6 1.503(11) . ? C5 H5A 0.9300 . ? C6 C7 1.489(11) . ? C7 C8 1.374(10) . ? C8 C9 1.382(9) . ? C8 H8A 0.9300 . ? C9 C8 1.382(9) 2 ? C9 H9A 0.9300 . ? C10 C11 1.513(12) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Hg1 N1 90.0(3) 2_656 . ? N1 Hg1 O2 90.2(2) 2_656 2_656 ? N1 Hg1 O2 110.3(2) . 2_656 ? N1 Hg1 O2 110.3(2) 2_656 . ? N1 Hg1 O2 90.2(2) . . ? O2 Hg1 O2 151.4(3) 2_656 . ? N1 Hg1 O3 143.8(2) 2_656 2_656 ? N1 Hg1 O3 98.4(2) . 2_656 ? O2 Hg1 O3 53.9(2) 2_656 2_656 ? O2 Hg1 O3 104.9(2) . 2_656 ? N1 Hg1 O3 98.4(2) 2_656 . ? N1 Hg1 O3 143.8(2) . . ? O2 Hg1 O3 104.9(2) 2_656 . ? O2 Hg1 O3 53.9(2) . . ? O3 Hg1 O3 95.3(3) 2_656 . ? N1 Hg1 C10 117.3(2) 2_656 2_656 ? N1 Hg1 C10 105.7(2) . 2_656 ? O2 Hg1 C10 27.2(2) 2_656 2_656 ? O2 Hg1 C10 129.4(3) . 2_656 ? O3 Hg1 C10 26.7(2) 2_656 2_656 ? O3 Hg1 C10 101.4(2) . 2_656 ? N1 Hg1 C10 105.7(2) 2_656 . ? N1 Hg1 C10 117.3(2) . . ? O2 Hg1 C10 129.4(3) 2_656 . ? O2 Hg1 C10 27.2(2) . . ? O3 Hg1 C10 101.4(2) 2_656 . ? O3 Hg1 C10 26.7(2) . . ? C10 Hg1 C10 117.9(3) 2_656 . ? C10 O2 Hg1 92.3(5) . . ? C10 O3 Hg1 90.8(5) . . ? C5 N1 C1 117.5(6) . . ? C5 N1 Hg1 123.4(5) . . ? C1 N1 Hg1 119.0(5) . . ? C7 N2 C7 116.2(8) . 2 ? N1 C1 C2 122.5(7) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C1 C2 C3 119.3(7) . . ? C1 C2 H2A 120.4 . . ? C3 C2 H2A 120.4 . . ? C4 C3 C2 118.9(7) . . ? C4 C3 H3A 120.5 . . ? C2 C3 H3A 120.5 . . ? C3 C4 C5 117.7(7) . . ? C3 C4 C6 123.3(6) . . ? C5 C4 C6 118.8(6) . . ? N1 C5 C4 124.0(6) . . ? N1 C5 H5A 118.0 . . ? C4 C5 H5A 118.0 . . ? O1 C6 C7 120.7(7) . . ? O1 C6 C4 120.1(7) . . ? C7 C6 C4 119.1(6) . . ? N2 C7 C8 123.8(7) . . ? N2 C7 C6 116.5(6) . . ? C8 C7 C6 119.7(7) . . ? C7 C8 C9 118.9(7) . . ? C7 C8 H8A 120.5 . . ? C9 C8 H8A 120.5 . . ? C8 C9 C8 118.4(10) 2 . ? C8 C9 H9A 120.8 2 . ? C8 C9 H9A 120.8 . . ? O3 C10 O2 122.9(8) . . ? O3 C10 C11 118.4(8) . . ? O2 C10 C11 118.6(8) . . ? O3 C10 Hg1 62.5(4) . . ? O2 C10 Hg1 60.5(4) . . ? C11 C10 Hg1 177.7(7) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Hg1 O2 C10 85.1(5) 2_656 . . . ? N1 Hg1 O2 C10 175.1(5) . . . . ? O2 Hg1 O2 C10 -48.1(5) 2_656 . . . ? O3 Hg1 O2 C10 -86.2(5) 2_656 . . . ? O3 Hg1 O2 C10 -0.5(5) . . . . ? C10 Hg1 O2 C10 -74.2(7) 2_656 . . . ? N1 Hg1 O3 C10 -108.5(5) 2_656 . . . ? N1 Hg1 O3 C10 -6.9(7) . . . . ? O2 Hg1 O3 C10 159.1(5) 2_656 . . . ? O2 Hg1 O3 C10 0.5(5) . . . . ? O3 Hg1 O3 C10 105.1(5) 2_656 . . . ? C10 Hg1 O3 C10 131.3(5) 2_656 . . . ? N1 Hg1 N1 C5 -42.6(5) 2_656 . . . ? O2 Hg1 N1 C5 47.6(6) 2_656 . . . ? O2 Hg1 N1 C5 -152.9(6) . . . . ? O3 Hg1 N1 C5 102.1(6) 2_656 . . . ? O3 Hg1 N1 C5 -146.9(5) . . . . ? C10 Hg1 N1 C5 75.8(6) 2_656 . . . ? C10 Hg1 N1 C5 -150.4(5) . . . . ? N1 Hg1 N1 C1 142.5(6) 2_656 . . . ? O2 Hg1 N1 C1 -127.3(5) 2_656 . . . ? O2 Hg1 N1 C1 32.3(5) . . . . ? O3 Hg1 N1 C1 -72.8(5) 2_656 . . . ? O3 Hg1 N1 C1 38.2(7) . . . . ? C10 Hg1 N1 C1 -99.0(5) 2_656 . . . ? C10 Hg1 N1 C1 34.8(6) . . . . ? C5 N1 C1 C2 -0.9(10) . . . . ? Hg1 N1 C1 C2 174.3(6) . . . . ? N1 C1 C2 C3 -0.6(12) . . . . ? C1 C2 C3 C4 1.5(11) . . . . ? C2 C3 C4 C5 -1.0(10) . . . . ? C2 C3 C4 C6 173.9(7) . . . . ? C1 N1 C5 C4 1.5(10) . . . . ? Hg1 N1 C5 C4 -173.4(5) . . . . ? C3 C4 C5 N1 -0.6(11) . . . . ? C6 C4 C5 N1 -175.7(7) . . . . ? C3 C4 C6 O1 -153.7(8) . . . . ? C5 C4 C6 O1 21.1(11) . . . . ? C3 C4 C6 C7 23.9(11) . . . . ? C5 C4 C6 C7 -161.3(7) . . . . ? C7 N2 C7 C8 1.2(5) 2 . . . ? C7 N2 C7 C6 -178.7(7) 2 . . . ? O1 C6 C7 N2 -144.2(7) . . . . ? C4 C6 C7 N2 38.2(9) . . . . ? O1 C6 C7 C8 35.9(11) . . . . ? C4 C6 C7 C8 -141.8(7) . . . . ? N2 C7 C8 C9 -2.4(10) . . . . ? C6 C7 C8 C9 177.5(6) . . . . ? C7 C8 C9 C8 1.1(5) . . . 2 ? Hg1 O3 C10 O2 -0.9(9) . . . . ? Hg1 O3 C10 C11 177.6(7) . . . . ? Hg1 O2 C10 O3 1.0(9) . . . . ? Hg1 O2 C10 C11 -177.6(7) . . . . ? N1 Hg1 C10 O3 77.1(5) 2_656 . . . ? N1 Hg1 C10 O3 175.4(5) . . . . ? O2 Hg1 C10 O3 -26.5(6) 2_656 . . . ? O2 Hg1 C10 O3 -179.1(8) . . . . ? O3 Hg1 C10 O3 -78.8(6) 2_656 . . . ? C10 Hg1 C10 O3 -56.4(5) 2_656 . . . ? N1 Hg1 C10 O2 -103.8(5) 2_656 . . . ? N1 Hg1 C10 O2 -5.5(6) . . . . ? O2 Hg1 C10 O2 152.6(4) 2_656 . . . ? O3 Hg1 C10 O2 100.3(5) 2_656 . . . ? O3 Hg1 C10 O2 179.1(8) . . . . ? C10 Hg1 C10 O2 122.7(6) 2_656 . . . ? N1 Hg1 C10 C11 -37(15) 2_656 . . . ? N1 Hg1 C10 C11 61(15) . . . . ? O2 Hg1 C10 C11 -141(15) 2_656 . . . ? O2 Hg1 C10 C11 67(15) . . . . ? O3 Hg1 C10 C11 167(15) 2_656 . . . ? O3 Hg1 C10 C11 -114(15) . . . . ? C10 Hg1 C10 C11 -171(15) 2_656 . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.291 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.158 #################################END###################